Background To study the ultra-trace simultaneous determination of drugs, the colorimetric method in combination with chemometrics can be used. Objective In this study, a simple, rapid, and sensitive UV-Vis spectrophotometric method using gold nanoparticles (AuNPs) was introduced for the simultaneous determination of ultra-trace amounts of Pilocarpine (PIL) and Timolol (TIM) in binary mixtures and biological sample. Methods AuNPs interacted with components and the aggregation mode of NPs occurred and finally, the color change of the solution (red to gray) was observed with the naked eye without the most modern and expensive instruments. The characterization of AuNPs was evaluated by transmission electron microscopy (TEM) and dynamic light scattering (DLS). Results The validation of the colorimetric way was studied in the concentration range of 100–800 and 100–600 μg/L with good linearity equal to 0.9772 and 0.9891 for PIL and TIM, respectively. The limit of detection (LOD) was found to be 165.00 and 92.40 μg/L, where the limit of quantitation (LOQ) was 500.00 and 280.00 μg/L for PIL and TIM, respectively. The effect of some factors such as interaction time, the concentration of components, and the volume of buffer on absorbance was investigated. Partial least squares (PLS) as an efficient multivariate calibration method was combined with colorimetry for the simultaneous determination of PIL and TIM in binary mixtures. The optimum number of latent variables was selected by k-fold cross-validation based on minimum mean square error prediction (MSEP) and the number of components equal to 1 with MSEP of 1.085 and 0.763 was considered for PIL and TIM, respectively. The mean recovery was obtained at 100.20% and 101.55% for PIL and TIM, respectively. Conclusion The colorimetric method can be introduced as a proper option for the simultaneous determination of components in pharmaceutical formulations and other samples. Highlights A colorimetric method using AuNPs was proposed. PLS method was coupled with a colorimetric method for the ultra-trace simultaneous estimation of PIL and TIM in binary mixtures. Ultra-trace amounts of PIL and TIM were also determined in biological sample. The proposed method is simple, fast and less expensive than chromatography methods.
背景 为研究超痕量药物的同时测定，可采用比色法结合化学计量学的方法。本研究采用金纳米粒子（AuNPs）建立了一种简单、快速、灵敏的紫外可见分光光度法，用于同时测定二元混合物和生物样品中的超痕量匹洛卡品（PIL）和噻吗洛尔（TIM）。这些方法使 AuNPs 与各种成分发生相互作用，并形成 NPs 的聚集模式，最后，不用最昂贵的现代仪器，用肉眼就能观察到溶液的颜色变化（从红色到灰色）。透射电子显微镜（TEM）和动态光散射（DLS）对 AuNPs 的特性进行了评估。结果 在 100-800 和 100-600 μg/L 的浓度范围内对比色法进行了验证，PIL 和 TIM 的线性分别为 0.9772 和 0.9891。PIL 和 TIM 的检出限（LOD）分别为 165.00 和 92.40 μg/L，定量限（LOQ）分别为 500.00 和 280.00 μg/L。研究了相互作用时间、成分浓度和缓冲液体积等因素对吸光度的影响。将偏最小二乘法（PLS）作为一种高效的多元定标方法与比色法相结合，用于同时测定二元混合物中的 PIL 和 TIM。根据最小均方误差预测法（MSEP），通过 k 倍交叉验证选择了最佳的潜变量数量，并认为 PIL 和 TIM 的成分数等于 1，MSEP 分别为 1.085 和 0.763。PIL 和 TIM 的平均回收率分别为 100.20% 和 101.55%。结论 该比色法可作为同时测定药物制剂和其他样品中成分的适当选择。要点 提出了一种使用 AuNPs 的比色法。将 PLS 法与比色法相结合，对二元混合物中的 PIL 和 TIM 进行超痕量同时测定。同时还测定了生物样品中 PIL 和 TIM 的超痕量含量。与色谱法相比，该方法简单、快速、成本低。
{"title":"Colorimetric Concurrent Determination of Ultra-Trace Amounts of Pilocarpine and Timolol as anti-Glaucoma Drugs in Binary Mixtures Using a Multivariate Calibration Approach Based on the Aggregation of Gold Nanoparticles","authors":"Asma Zanjani, Mahmoud Reza Sohrabi, Hassan Kabiri Fard","doi":"10.1093/jaoacint/qsae030","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae030","url":null,"abstract":"Background To study the ultra-trace simultaneous determination of drugs, the colorimetric method in combination with chemometrics can be used. Objective In this study, a simple, rapid, and sensitive UV-Vis spectrophotometric method using gold nanoparticles (AuNPs) was introduced for the simultaneous determination of ultra-trace amounts of Pilocarpine (PIL) and Timolol (TIM) in binary mixtures and biological sample. Methods AuNPs interacted with components and the aggregation mode of NPs occurred and finally, the color change of the solution (red to gray) was observed with the naked eye without the most modern and expensive instruments. The characterization of AuNPs was evaluated by transmission electron microscopy (TEM) and dynamic light scattering (DLS). Results The validation of the colorimetric way was studied in the concentration range of 100–800 and 100–600 μg/L with good linearity equal to 0.9772 and 0.9891 for PIL and TIM, respectively. The limit of detection (LOD) was found to be 165.00 and 92.40 μg/L, where the limit of quantitation (LOQ) was 500.00 and 280.00 μg/L for PIL and TIM, respectively. The effect of some factors such as interaction time, the concentration of components, and the volume of buffer on absorbance was investigated. Partial least squares (PLS) as an efficient multivariate calibration method was combined with colorimetry for the simultaneous determination of PIL and TIM in binary mixtures. The optimum number of latent variables was selected by k-fold cross-validation based on minimum mean square error prediction (MSEP) and the number of components equal to 1 with MSEP of 1.085 and 0.763 was considered for PIL and TIM, respectively. The mean recovery was obtained at 100.20% and 101.55% for PIL and TIM, respectively. Conclusion The colorimetric method can be introduced as a proper option for the simultaneous determination of components in pharmaceutical formulations and other samples. Highlights A colorimetric method using AuNPs was proposed. PLS method was coupled with a colorimetric method for the ultra-trace simultaneous estimation of PIL and TIM in binary mixtures. Ultra-trace amounts of PIL and TIM were also determined in biological sample. The proposed method is simple, fast and less expensive than chromatography methods.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":"43 1","pages":""},"PeriodicalIF":1.6,"publicationDate":"2024-04-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140578514","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-04-03DOI: 10.1093/jaoacint/qsae029
Anthony Kovalenko, Dominique Stutts, Patrick J Gray
Background An interlaboratory study was conducted at the U.S. Food and Drug Administration’s (FDA) Northeast Food and Feed Laboratory (NFFL) and the Center for Food Safety and Applied Nutrition (CFSAN) with the purpose to expand FDA Elemental Analysis Manual (EAM) method 4.7 (Inductively Coupled Plasma-Mass Spectrometric Determination of Arsenic, Cadmium, Chromium, Lead, Mercury, and Other Elements in Food Using Microwave Assisted Digestion) to include new analytes (1). Objective The goal of the study was to demonstrate the performance of FDA EAM method 4.7 when analyzing new analytes cobalt (Co), strontium (Sr), thallium (Tl), tin (Sn), uranium (U) and vanadium (V). This analyte extension method validation of EAM 4.7 for six additional elements, Co, Sr, Tl, Sn, U and V followed all guidelines for a Level 2 or single laboratory validation and met all acceptance criteria for analyte extensions as per the Guidelines for the Validation of Chemical Methods (3). Method As per EAM 4.7 (1), this study followed the procedures and used specified equipment operated under recommended conditions. The analyte extension method validation was performed per protocol and with no deviations. Results All quality control (QC) requirements for this analyte extension method validation of EAM 4.7 passed as evidenced by the analytical data. The results presented demonstrate accuracy, linearity and precision by successful analyses of method blanks, matrix spikes, unfortified test samples and reference materials. The data analyzed met each of the validation requirements for each analyte in all representative matrices. Conclusion The study showed that the new analytes performed satisfactorily using EAM 4.7 for total acidic extractable elemental analysis of food according to FDA’s guidelines (3). Highlights The method met or exceeded the performance criteria.
背景 美国食品和药物管理局（FDA）东北食品和饲料实验室（NFFL）以及食品安全和应用营养中心（CFSAN）开展了一项实验室间研究，目的是扩展 FDA 元素分析手册（EAM）方法 4.7（使用微波辅助消化法，电感耦合等离子体-质谱法测定食品中的砷、镉、铬、铅、汞和其他元素），以纳入新的分析物(1)。这项研究的目的是证明 FDA EAM 方法 4.7 在分析新的分析物钴（Co）、锶（Sr）、铊 （Tl）、锡（Sn）、铀（U）和钒（V）时的性能。对 EAM 4.7 进行的钴 (Co)、锶 (Sr)、铊 (Tl)、锡 (Sn)、铀 (U) 和钒 (V) 六种新增元素的分析物扩展方法验证，遵循了二级或单一实验室验证的所有准则，并符合《化学方法验证准则》(3) 规定的分析物扩展的所有验收标准。方法 根据 EAM 4.7 (1)，本研究遵循了相关程序，并使用了在建议条件下运行的指定设备。分析物扩展方法验证是按照规程进行的，没有任何偏差。结果 从分析数据来看，EAM 4.7 中关于被分析物扩展方法验证的所有质量控制 (QC) 要求均已通过。通过对方法空白、基质尖峰、未强化测试样品和参考材料的成功分析，结果表明了准确度、线性度和精密度。分析数据符合所有代表性基质中每种分析物的验证要求。结论 研究表明，使用 EAM 4.7 对食品进行总酸性可萃取元素分析时，新分析物的性能令人满意，符合 FDA 的指导原则 (3)。亮点 该方法达到或超过了性能标准。
{"title":"Analyte Extension Method Validation of Elemental Analysis Manual Method 4.7 for Six Additional Elements, Cobalt (Co), Strontium (Sr), Thallium (Tl), Tin (Sn), Uranium (U) and Vanadium (V)","authors":"Anthony Kovalenko, Dominique Stutts, Patrick J Gray","doi":"10.1093/jaoacint/qsae029","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae029","url":null,"abstract":"Background An interlaboratory study was conducted at the U.S. Food and Drug Administration’s (FDA) Northeast Food and Feed Laboratory (NFFL) and the Center for Food Safety and Applied Nutrition (CFSAN) with the purpose to expand FDA Elemental Analysis Manual (EAM) method 4.7 (Inductively Coupled Plasma-Mass Spectrometric Determination of Arsenic, Cadmium, Chromium, Lead, Mercury, and Other Elements in Food Using Microwave Assisted Digestion) to include new analytes (1). Objective The goal of the study was to demonstrate the performance of FDA EAM method 4.7 when analyzing new analytes cobalt (Co), strontium (Sr), thallium (Tl), tin (Sn), uranium (U) and vanadium (V). This analyte extension method validation of EAM 4.7 for six additional elements, Co, Sr, Tl, Sn, U and V followed all guidelines for a Level 2 or single laboratory validation and met all acceptance criteria for analyte extensions as per the Guidelines for the Validation of Chemical Methods (3). Method As per EAM 4.7 (1), this study followed the procedures and used specified equipment operated under recommended conditions. The analyte extension method validation was performed per protocol and with no deviations. Results All quality control (QC) requirements for this analyte extension method validation of EAM 4.7 passed as evidenced by the analytical data. The results presented demonstrate accuracy, linearity and precision by successful analyses of method blanks, matrix spikes, unfortified test samples and reference materials. The data analyzed met each of the validation requirements for each analyte in all representative matrices. Conclusion The study showed that the new analytes performed satisfactorily using EAM 4.7 for total acidic extractable elemental analysis of food according to FDA’s guidelines (3). Highlights The method met or exceeded the performance criteria.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":"66 1","pages":""},"PeriodicalIF":1.6,"publicationDate":"2024-04-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140578306","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Background Camptothecin is a potent anti-cancer drug used for the treatment of various cancers. Objective The goal of this research investigation was to develop and validate a new stability indicating HPLC technique for the quantitative assessment of camptothecin in in-house developed mesoporous silica nanoparticles, a novel nanoformulation matrix for the treatment of cancer. Method The Waters Inertsil® HPLC column (C18) was used for the chromatographic separation, with a flow rate of 1 mL/min, a column oven temperature of 40 °C, an injection volume of 10 µL, a detection wavelength of 216 nm, and a 10 min runtime overall. An isocratic blend of phosphate buffer (10 mM, pH7.0) and acetonitrile (60:40 v/v) served as the mobile phase. Various stress conditions including acid, alkali, oxidative, photolytic, thermal, and humidity environments were tested for the quantitative estimation of the camptothecin through the proposed method. Results The results demonstrated that the proposed method is specific (peak purity ≥ 0.999), accurate (99.69—100.64% w/w), precise (%RSD < 2.0), and sensitive (LOD—0.17 µg and LOQ—0.56 µg) in accordance with ICH guideline Q2(R1). Any unidentified degradation products did not interfere with the drug's estimation. Furthermore, the current method of analysis has eliminated any excipient interference from the matrix effect caused by the numerous excipients of the formulation matrix. Conclusions To quantify camptothecin for routine assay purposes, this research work offers a novel and straightforward HPLC methodology with optimized chromatographic parameters, contributing to the research and development community while ensuring an appropriate and efficient use of the drug through a variety of nanoformulation for cancer treatment. Highlights Stability-indicating HPLC method was found to be specific and suitable for routine analysis of camptothecin. The absence of any interference from excipients was confirmed by forced degradation studies.
{"title":"A Robust HPLC Approach for Quantitation of Camptothecin in Mesoporous Silica Nanoparticles Matrix and in the Presence of Its Degradation Products","authors":"Richa Dave, Neel Savaliya, Ashish Dobariya, Rashmin Patel, Mrunali Patel","doi":"10.1093/jaoacint/qsae013","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae013","url":null,"abstract":"Background Camptothecin is a potent anti-cancer drug used for the treatment of various cancers. Objective The goal of this research investigation was to develop and validate a new stability indicating HPLC technique for the quantitative assessment of camptothecin in in-house developed mesoporous silica nanoparticles, a novel nanoformulation matrix for the treatment of cancer. Method The Waters Inertsil® HPLC column (C18) was used for the chromatographic separation, with a flow rate of 1 mL/min, a column oven temperature of 40 °C, an injection volume of 10 µL, a detection wavelength of 216 nm, and a 10 min runtime overall. An isocratic blend of phosphate buffer (10 mM, pH7.0) and acetonitrile (60:40 v/v) served as the mobile phase. Various stress conditions including acid, alkali, oxidative, photolytic, thermal, and humidity environments were tested for the quantitative estimation of the camptothecin through the proposed method. Results The results demonstrated that the proposed method is specific (peak purity ≥ 0.999), accurate (99.69—100.64% w/w), precise (%RSD &lt; 2.0), and sensitive (LOD—0.17 µg and LOQ—0.56 µg) in accordance with ICH guideline Q2(R1). Any unidentified degradation products did not interfere with the drug's estimation. Furthermore, the current method of analysis has eliminated any excipient interference from the matrix effect caused by the numerous excipients of the formulation matrix. Conclusions To quantify camptothecin for routine assay purposes, this research work offers a novel and straightforward HPLC methodology with optimized chromatographic parameters, contributing to the research and development community while ensuring an appropriate and efficient use of the drug through a variety of nanoformulation for cancer treatment. Highlights Stability-indicating HPLC method was found to be specific and suitable for routine analysis of camptothecin. The absence of any interference from excipients was confirmed by forced degradation studies.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":"21 1","pages":""},"PeriodicalIF":1.6,"publicationDate":"2024-02-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139969190","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-02-23DOI: 10.1093/jaoacint/qsae014
Lijun Hu, Guodong Zhang
Background For pathogen detection in food, there are occasions where samples cannot be processed immediately after selective enrichment or need to be reexamined days/weeks later for confirmation or retest. Objective This study aimed to investigate the effect of different prolonged period of storage of selective enrichments of food at 4 ± 2 °C and room temperature (20—22 °C) on the detection and isolation of Salmonella. Methods This study included two experiments involving 34 types of foods to compare the effect of 4 ± 2 °C and room temperature storage on the detection of Salmonella in 204 selective enrichments [Rappaport-Vassiliadis (RV) and Tetrathionate (TT) broths] during a 42-day storage (Experiment I); and to monitor the survival of Salmonella in 300 selective enrichments (RV and TT) with different pre-enrichment broths [Lactose broth (LB) or Buffered peptone water broth (BPW)], stored at 4 °C for 60 days (Experiment II). All the samples were subjected to Salmonella analysis following FDA BAM method. Results During multiple samplings, the positive detection rate for Salmonella remained consistent through Day 42 after selective enrichment, irrespective of Salmonella serotype, storage temperature, pre-enrichment broth, or selective enrichment broth in both Experiment I and II. However, on Day 60 sampling in Experiment II, seven previously positive results turned to negatives. This data indicated that storage of RV and TT enrichments at 4 ± 2 °C or room temperature for up to 42 days after selective enrichment did not compromise the detection of Salmonella in the tested food categories, regardless of Salmonella serotypes and the broths used for pre-enrichment and selective enrichment. Conclusion At least for the specific food types studied in this experiment, the recovery of Salmonella from selective enrichments could be postponed for a limited period of time (e.g., < 42 days) if needed without adversely affecting the test results. However, the delayed analysis of TT and RV enrichments does pose a risk of reduced detection sensitivity, as evidenced by the seven negative results on Day 60 compared to previous positives. We do not recommend or endorse delaying the analysis of TT and RV enrichments. Highlights In the food matrices investigated in this experiment, the plating and isolation of Salmonella from selective TT and RV enrichments stored at 4 ± 2 °C or room temperature could be deferred for a period (up to 42 days) without any negative effect on the test results, if necessary.
{"title":"Effect of selective enrichment storage temperature and duration time on the detection of Salmonella in food","authors":"Lijun Hu, Guodong Zhang","doi":"10.1093/jaoacint/qsae014","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae014","url":null,"abstract":"Background For pathogen detection in food, there are occasions where samples cannot be processed immediately after selective enrichment or need to be reexamined days/weeks later for confirmation or retest. Objective This study aimed to investigate the effect of different prolonged period of storage of selective enrichments of food at 4 ± 2 °C and room temperature (20—22 °C) on the detection and isolation of Salmonella. Methods This study included two experiments involving 34 types of foods to compare the effect of 4 ± 2 °C and room temperature storage on the detection of Salmonella in 204 selective enrichments [Rappaport-Vassiliadis (RV) and Tetrathionate (TT) broths] during a 42-day storage (Experiment I); and to monitor the survival of Salmonella in 300 selective enrichments (RV and TT) with different pre-enrichment broths [Lactose broth (LB) or Buffered peptone water broth (BPW)], stored at 4 °C for 60 days (Experiment II). All the samples were subjected to Salmonella analysis following FDA BAM method. Results During multiple samplings, the positive detection rate for Salmonella remained consistent through Day 42 after selective enrichment, irrespective of Salmonella serotype, storage temperature, pre-enrichment broth, or selective enrichment broth in both Experiment I and II. However, on Day 60 sampling in Experiment II, seven previously positive results turned to negatives. This data indicated that storage of RV and TT enrichments at 4 ± 2 °C or room temperature for up to 42 days after selective enrichment did not compromise the detection of Salmonella in the tested food categories, regardless of Salmonella serotypes and the broths used for pre-enrichment and selective enrichment. Conclusion At least for the specific food types studied in this experiment, the recovery of Salmonella from selective enrichments could be postponed for a limited period of time (e.g., &lt; 42 days) if needed without adversely affecting the test results. However, the delayed analysis of TT and RV enrichments does pose a risk of reduced detection sensitivity, as evidenced by the seven negative results on Day 60 compared to previous positives. We do not recommend or endorse delaying the analysis of TT and RV enrichments. Highlights In the food matrices investigated in this experiment, the plating and isolation of Salmonella from selective TT and RV enrichments stored at 4 ± 2 °C or room temperature could be deferred for a period (up to 42 days) without any negative effect on the test results, if necessary.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":"41 1","pages":""},"PeriodicalIF":1.6,"publicationDate":"2024-02-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139968945","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-02-04DOI: 10.1093/jaoacint/qsae010
Mohammad Kashif, Swati Acharya, Adila Khalil
Since 2019 the world is in a combat with the highly contagious disease COVID-19 that is caused by the rapid transmission of SARS-CoV-2 virus (severe acute respiratory syndrome- coronavirus-2). Detection of this disease in an early stage helps to control its spread and management. To combat this epidemic with one-time effective medication improved quick analytical procedures must be developed and validated. The requirement of accurate and precise analytical methods for the diagnosis of the virus and antibodies in infected patients has been a matter of concern. The global impact of this virus has motivated scientists and researchers to investigate and develop various analytical diagnostic techniques. This review includes the study of standard methods which are reliable and accredited for the analytical recognition of the said virus. For early detection of SARS-CoV-2 RNA, RT-PCR is an accurate method among other methods and thus, considered as “gold standard” technique. Here, we outline the most extensively used analytical methods for diagnosing COVID-19, along with a brief description of each technique and its analytical aspects/perspective.
{"title":"Molecular Interactions Leading to the Advancement in the Techniques for COVID-19 Detection: A Review","authors":"Mohammad Kashif, Swati Acharya, Adila Khalil","doi":"10.1093/jaoacint/qsae010","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae010","url":null,"abstract":"Since 2019 the world is in a combat with the highly contagious disease COVID-19 that is caused by the rapid transmission of SARS-CoV-2 virus (severe acute respiratory syndrome- coronavirus-2). Detection of this disease in an early stage helps to control its spread and management. To combat this epidemic with one-time effective medication improved quick analytical procedures must be developed and validated. The requirement of accurate and precise analytical methods for the diagnosis of the virus and antibodies in infected patients has been a matter of concern. The global impact of this virus has motivated scientists and researchers to investigate and develop various analytical diagnostic techniques. This review includes the study of standard methods which are reliable and accredited for the analytical recognition of the said virus. For early detection of SARS-CoV-2 RNA, RT-PCR is an accurate method among other methods and thus, considered as “gold standard” technique. Here, we outline the most extensively used analytical methods for diagnosing COVID-19, along with a brief description of each technique and its analytical aspects/perspective.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":"116 1","pages":""},"PeriodicalIF":1.6,"publicationDate":"2024-02-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139677475","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Background The Eco-friendly analytical technique was developed for intention of preserving the environment by using green chemistry principles. Pemetrexed is folate analogue indicated for treatment of advanced lung cancer. Objective Development of Green Stability indicating HPLC method for quantification of Pemetrexed (Ditromethamine) impurities in API and parenteral dosage form. Method Chromatographic separation was achieved by using Zorbax SB C18 column (150 mm x 4.6 mm inner diameter, 3.5 µ particle size) with perchlorate buffer (pH 3.0 ± 0.1, 50 mM) as a mobile phase-A and Acetonitrile—perchlorate buffer (90 + 10, v/v) as a mobile phase-B at a flow rate of 0.8 mL/minute with column temperature 40 °C ± 0.5 °C. All analytes were well resolved by gradient elution with total run time of 75 minutes and detection wavelength at UV 230 nm. Results The RP-HPLC method is capable to resolve all the degradation and process impurities for Pemetrexed Ditromethamine API and parenteral dosage form. The related compounds method was validated in accordance with ICH Q2(R1) and USP <1225> guidelines, found to be accurate, specific, precise, linear, robust and stability indicating. The precision and intermediate results shown the below < 5% CV values for all the impurities. The accuracy of all the impurities were found to be between 90% and 110%. The linearity of regression co-efficient values for all the impurities were found to be more than 0.999. Conclusion The proposed related compounds method is found suitable for the determination of process and degradation impurities of commercial formulations, stability samples in quality control analysis for Pemetrexed Ditromethamine (PDT) API and drug product. Highlights The developed liquid chromatographic method greenness and eco-friendliness were assessed by using (GAPI) green analytical procedure index, (AGREE) analytical greenness tool, and found to be green. Pemetrexed Ditromethamine detoxification procedure also developed to protect from environment pollution.
{"title":"Eco-Friendly Stability-Indicating HPLC Method for Related Compounds in Pemetrexed Ditromethamine (Antineoplastic Agent) for Injection","authors":"Arjuna Rao Nekkalapudi, Srinivasu Navuluri, Sreenivas Pippalla","doi":"10.1093/jaoacint/qsae008","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae008","url":null,"abstract":"Background The Eco-friendly analytical technique was developed for intention of preserving the environment by using green chemistry principles. Pemetrexed is folate analogue indicated for treatment of advanced lung cancer. Objective Development of Green Stability indicating HPLC method for quantification of Pemetrexed (Ditromethamine) impurities in API and parenteral dosage form. Method Chromatographic separation was achieved by using Zorbax SB C18 column (150 mm x 4.6 mm inner diameter, 3.5 µ particle size) with perchlorate buffer (pH 3.0 ± 0.1, 50 mM) as a mobile phase-A and Acetonitrile—perchlorate buffer (90 + 10, v/v) as a mobile phase-B at a flow rate of 0.8 mL/minute with column temperature 40 °C ± 0.5 °C. All analytes were well resolved by gradient elution with total run time of 75 minutes and detection wavelength at UV 230 nm. Results The RP-HPLC method is capable to resolve all the degradation and process impurities for Pemetrexed Ditromethamine API and parenteral dosage form. The related compounds method was validated in accordance with ICH Q2(R1) and USP &lt;1225&gt; guidelines, found to be accurate, specific, precise, linear, robust and stability indicating. The precision and intermediate results shown the below &lt; 5% CV values for all the impurities. The accuracy of all the impurities were found to be between 90% and 110%. The linearity of regression co-efficient values for all the impurities were found to be more than 0.999. Conclusion The proposed related compounds method is found suitable for the determination of process and degradation impurities of commercial formulations, stability samples in quality control analysis for Pemetrexed Ditromethamine (PDT) API and drug product. Highlights The developed liquid chromatographic method greenness and eco-friendliness were assessed by using (GAPI) green analytical procedure index, (AGREE) analytical greenness tool, and found to be green. Pemetrexed Ditromethamine detoxification procedure also developed to protect from environment pollution.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":"12 1","pages":""},"PeriodicalIF":1.6,"publicationDate":"2024-02-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139677347","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-01-11DOI: 10.1093/jaoacint/qsae004
Dilek Çam Derin, Enes Gültekin, Elif Gündüz, Barış Otlu
Background SARS-CoV-2 is a threat for humanity. Both the Spike (S) protein and its receptor binding domain (sRBD) are extensively used for the rapid detection. Although real time reverse transcription polymerase chain reaction (rRT-PCR) is mostly used method for the molecular detection of SARS-CoV-2, rapid assays for antigenic detection is always needed. Lateral flow assays (LFAs) are the most commonly used tests for this purpose and aptamers having stability and long shelf life are used as capture reagents. Objective This study aimed to develop the LFAs based on the aptamer pairs for the antigenic detection of SARS-CoV-2 with naked eye. Methods Gold nanoparticles (AuNPs) were used as label and six sandwich models by three different aptamers were prepared using 4 μM and 8 μM probes and two kinds of membranes for developing the LFAs. Results 8 μM probe concentration and M2 membrane showed the best recognition of both the synthetic sRBD and SARS-CoV-2 coming from the naso/oropharingeal swabs by designed LFAs as 100% sensitivity and 93,3% specifity compared to the antibody detecting LFAs. Conclusions Our developed strip assays based on aptamer pairs recognized the target, directly in a 5-6 minutes with naked eye. It was also concluded that aptamer pairs, membrane types, assay buffers and probe concentrations have significant role in the detection of SARS-CoV-2 by LFAs. Highlights The detection of SARS-CoV-2 in clinical samples was demonstrated with the best aptamer pairs, sensitively and selectively among the designed 6 aptamer pairs for LFAs. Developed LFAs can be an alternative method to the conventional antibody based LFAs for SARS-CoV-2 detection.
{"title":"Comparison of 6 aptamer-aptamer pairs on rapid detection of SARS-CoV-2 by lateral flow assay","authors":"Dilek Çam Derin, Enes Gültekin, Elif Gündüz, Barış Otlu","doi":"10.1093/jaoacint/qsae004","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae004","url":null,"abstract":"Background SARS-CoV-2 is a threat for humanity. Both the Spike (S) protein and its receptor binding domain (sRBD) are extensively used for the rapid detection. Although real time reverse transcription polymerase chain reaction (rRT-PCR) is mostly used method for the molecular detection of SARS-CoV-2, rapid assays for antigenic detection is always needed. Lateral flow assays (LFAs) are the most commonly used tests for this purpose and aptamers having stability and long shelf life are used as capture reagents. Objective This study aimed to develop the LFAs based on the aptamer pairs for the antigenic detection of SARS-CoV-2 with naked eye. Methods Gold nanoparticles (AuNPs) were used as label and six sandwich models by three different aptamers were prepared using 4 μM and 8 μM probes and two kinds of membranes for developing the LFAs. Results 8 μM probe concentration and M2 membrane showed the best recognition of both the synthetic sRBD and SARS-CoV-2 coming from the naso/oropharingeal swabs by designed LFAs as 100% sensitivity and 93,3% specifity compared to the antibody detecting LFAs. Conclusions Our developed strip assays based on aptamer pairs recognized the target, directly in a 5-6 minutes with naked eye. It was also concluded that aptamer pairs, membrane types, assay buffers and probe concentrations have significant role in the detection of SARS-CoV-2 by LFAs. Highlights The detection of SARS-CoV-2 in clinical samples was demonstrated with the best aptamer pairs, sensitively and selectively among the designed 6 aptamer pairs for LFAs. Developed LFAs can be an alternative method to the conventional antibody based LFAs for SARS-CoV-2 detection.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":"1 1","pages":""},"PeriodicalIF":1.6,"publicationDate":"2024-01-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139462978","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-01-10DOI: 10.1093/jaoacint/qsae002
F Codony, G Agustí, L Barreto, D Asensio
Background When detecting Salmonella spp. in food samples, unlike with culture-based procedures where there are solid standards, PCR techniques are generally dominated by commercial solutions, often backed by the conformity of reference organizations, and based on rigorous validation studies. The few independent standards that exist are not subject to revision and improvement to the same extent as the manufacturer's methods. Moreover, since commercial networks do not promote them, they are less implemented in everyday practice. The German standard DIN 10135 is an example of this. In this method, before PCR detection, a primary enrichment (16–20 h) followed by a secondary selective enrichment of at least 6 hours is needed. Nevertheless, it allows the possibility of only apply the first step if evidence of their correct operation is provided. Objective To evaluate how necessary is the secondary enrichment for DIN 10135 standard. Methods Short and complete enrichment steps were compared in the context of the evaluation of the limit of detection for 11 types of food. Additionally, a blind assay was performed with 75 food samples. Results The data show that a simple primary enrichment may be sufficient and that the second selective enrichment with the tested matrices would not be strictly essential. The blind study obtained a 98.6% of trueness and precision of 100%. Conclusions At least for the end consumer products, a secondary enrichment of 6 hours is not necessary for all the products tested. Highlights In the context of the DIN 10135 standard, the primary enrichment (16–20 h, 37 ± 1 °C) can be enough for detecting Salmonella spp.
{"title":"Relevance of Secondary Enrichment in the Detection of Salmonella Spp in Food Samples by qPCR according to DIN 10135","authors":"F Codony, G Agustí, L Barreto, D Asensio","doi":"10.1093/jaoacint/qsae002","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae002","url":null,"abstract":"Background When detecting Salmonella spp. in food samples, unlike with culture-based procedures where there are solid standards, PCR techniques are generally dominated by commercial solutions, often backed by the conformity of reference organizations, and based on rigorous validation studies. The few independent standards that exist are not subject to revision and improvement to the same extent as the manufacturer's methods. Moreover, since commercial networks do not promote them, they are less implemented in everyday practice. The German standard DIN 10135 is an example of this. In this method, before PCR detection, a primary enrichment (16–20 h) followed by a secondary selective enrichment of at least 6 hours is needed. Nevertheless, it allows the possibility of only apply the first step if evidence of their correct operation is provided. Objective To evaluate how necessary is the secondary enrichment for DIN 10135 standard. Methods Short and complete enrichment steps were compared in the context of the evaluation of the limit of detection for 11 types of food. Additionally, a blind assay was performed with 75 food samples. Results The data show that a simple primary enrichment may be sufficient and that the second selective enrichment with the tested matrices would not be strictly essential. The blind study obtained a 98.6% of trueness and precision of 100%. Conclusions At least for the end consumer products, a secondary enrichment of 6 hours is not necessary for all the products tested. Highlights In the context of the DIN 10135 standard, the primary enrichment (16–20 h, 37 ± 1 °C) can be enough for detecting Salmonella spp.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":"12 1","pages":""},"PeriodicalIF":1.6,"publicationDate":"2024-01-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139462938","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-01-09DOI: 10.1093/jaoacint/qsae005
Harold A Prada-Ramírez, Juan Pablo Montes-Tamara, Eduardo A Rico-Jimenez, Juan Camilo Fonseca
Background Holding times for raw materials are relevant, since they enable us to understand the allowable time that a raw material can be kept under ideal storage conditions before the start of the manufacturing process without its quality attributes being affected. The quantification of water activity can be used as an indicator of the microbiological, physicochemical, and organoleptic stability of a specimen, since low water activity retards autohydrolysis and microbiological growth. Objective The main purpose of this investigation was to test the stability of powdered raw materials for a maximum holding time of 8 days through water activity measurements. Thus microbiological, physicochemical, and organoleptic measurements were carried out in parallel and simultaneously in order to experimentally establish a relationship between the status of the water activity of processed raw materials and the microbiological, physicochemical, and organoleptic results. Results The raw materials were stored for a maximum holding time of 8 days, in accordance with USP monographs. For all the raw materials tested, water activity measurements were performed using the dew point chilled-mirror method on days 0, 3, and 8. On days 0 and 8, microbiological, physicochemical, and organoleptic assessments were performed. It was established that under these storage conditions, the processed raw materials exhibited water activity below 0.60 during the entire holding time. However, there were statistically significant differences in water activity levels between days 0, 3, and 8 (ANOVA P < 0.05). Despite observing statistically significant differences between days, the microbiological, physicochemical, and organoleptic features were within specification at those water activity levels, below 0.60. Conclusion Water activity below 0.60 does not allow the growth of microorganisms, and the organoleptic and physicochemical features remain unperturbed. The results indicate that water activity can be used as an indicator of the microbiological load and chemical stability of the raw materials tested.
{"title":"Stability Study Through Water Activity Measurements for Dispensed Powdered Raw Materials","authors":"Harold A Prada-Ramírez, Juan Pablo Montes-Tamara, Eduardo A Rico-Jimenez, Juan Camilo Fonseca","doi":"10.1093/jaoacint/qsae005","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae005","url":null,"abstract":"Background Holding times for raw materials are relevant, since they enable us to understand the allowable time that a raw material can be kept under ideal storage conditions before the start of the manufacturing process without its quality attributes being affected. The quantification of water activity can be used as an indicator of the microbiological, physicochemical, and organoleptic stability of a specimen, since low water activity retards autohydrolysis and microbiological growth. Objective The main purpose of this investigation was to test the stability of powdered raw materials for a maximum holding time of 8 days through water activity measurements. Thus microbiological, physicochemical, and organoleptic measurements were carried out in parallel and simultaneously in order to experimentally establish a relationship between the status of the water activity of processed raw materials and the microbiological, physicochemical, and organoleptic results. Results The raw materials were stored for a maximum holding time of 8 days, in accordance with USP monographs. For all the raw materials tested, water activity measurements were performed using the dew point chilled-mirror method on days 0, 3, and 8. On days 0 and 8, microbiological, physicochemical, and organoleptic assessments were performed. It was established that under these storage conditions, the processed raw materials exhibited water activity below 0.60 during the entire holding time. However, there were statistically significant differences in water activity levels between days 0, 3, and 8 (ANOVA P &lt; 0.05). Despite observing statistically significant differences between days, the microbiological, physicochemical, and organoleptic features were within specification at those water activity levels, below 0.60. Conclusion Water activity below 0.60 does not allow the growth of microorganisms, and the organoleptic and physicochemical features remain unperturbed. The results indicate that water activity can be used as an indicator of the microbiological load and chemical stability of the raw materials tested.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":"7 1","pages":""},"PeriodicalIF":1.6,"publicationDate":"2024-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139462985","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-01-09DOI: 10.1093/jaoacint/qsae001
Thierry Bénet, Nathalie Frei, Véronique Spichtig, Denis Cuany, Sean Austin
Background Human milk oligosaccharides (HMOs) are important components of breast milk and may be responsible for some of the benefits of breastfeeding, including resistance to infections and the development of a healthy gut microbiota. Selected HMOs are now available for addition to infant formula, and suitable methods to control the dosing rate are needed. Objective To develop and validate a suitable method for the analysis of HMOs in infant formula. Method A method was developed for the determination of seven human milk oligosaccharides (2’-fucosyllactose, 3-fucosyllactose, 3’-sialyllactose, 6’-sialyllactose (6’SL), 2’,3-difucosyllactose, lacto-N-tetraose (LNT), lacto-N-neotetraose (LNnT)) in infant formula and adult nutritionals. The oligosaccharides are labelled at their reducing end with 2-aminobenzamide, separated by liquid chromatography and detected using a fluorescence detector. Maltodextrins are enzymatically hydrolyzed before analysis to prevent potential interference, likewise an optional β-galactosidase treatment can be used to remove β-galactooligosaccharides. Fructooligosaccharides or polydextrose do not generally interfere with the analysis. Results The method has been validated in a single laboratory on infant formula and adult nutritionals. The seven HMOs were spiked in to eight matrices at three or four spike levels giving a total of 176 data points. Recoveries were in the range 90.9–109% in all cases except at the lowest spike level in one matrix (elemental formula), where the LNT recovery was 113%, the LNnT recovery was 111% and the 6’SL recovery was 121%. Relative repeatabilities (RSD(r)) were in the range 0.1–4.2%. The performance is generally within the requirements outlined in the Standard Method Performance Requirements (SMPR®) published by AOAC International. Conclusions The method developed is suitable for the determination of seven HMOs in infant formula and demonstrated good performance during single laboratory validation. Highlights A method has been developed which is suitable for the determination of seven HMOs in infant formula.
{"title":"Determination of Seven Human Milk Oligosaccharides (HMO) in Infant Formula and Adult Nutritionals: First Action 2022.07","authors":"Thierry Bénet, Nathalie Frei, Véronique Spichtig, Denis Cuany, Sean Austin","doi":"10.1093/jaoacint/qsae001","DOIUrl":"https://doi.org/10.1093/jaoacint/qsae001","url":null,"abstract":"Background Human milk oligosaccharides (HMOs) are important components of breast milk and may be responsible for some of the benefits of breastfeeding, including resistance to infections and the development of a healthy gut microbiota. Selected HMOs are now available for addition to infant formula, and suitable methods to control the dosing rate are needed. Objective To develop and validate a suitable method for the analysis of HMOs in infant formula. Method A method was developed for the determination of seven human milk oligosaccharides (2’-fucosyllactose, 3-fucosyllactose, 3’-sialyllactose, 6’-sialyllactose (6’SL), 2’,3-difucosyllactose, lacto-N-tetraose (LNT), lacto-N-neotetraose (LNnT)) in infant formula and adult nutritionals. The oligosaccharides are labelled at their reducing end with 2-aminobenzamide, separated by liquid chromatography and detected using a fluorescence detector. Maltodextrins are enzymatically hydrolyzed before analysis to prevent potential interference, likewise an optional β-galactosidase treatment can be used to remove β-galactooligosaccharides. Fructooligosaccharides or polydextrose do not generally interfere with the analysis. Results The method has been validated in a single laboratory on infant formula and adult nutritionals. The seven HMOs were spiked in to eight matrices at three or four spike levels giving a total of 176 data points. Recoveries were in the range 90.9–109% in all cases except at the lowest spike level in one matrix (elemental formula), where the LNT recovery was 113%, the LNnT recovery was 111% and the 6’SL recovery was 121%. Relative repeatabilities (RSD(r)) were in the range 0.1–4.2%. The performance is generally within the requirements outlined in the Standard Method Performance Requirements (SMPR®) published by AOAC International. Conclusions The method developed is suitable for the determination of seven HMOs in infant formula and demonstrated good performance during single laboratory validation. Highlights A method has been developed which is suitable for the determination of seven HMOs in infant formula.","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":"76 3","pages":""},"PeriodicalIF":1.6,"publicationDate":"2024-01-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139462850","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"农林科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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