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Determination of Gemcitabine and Sorafenib in Spiked Human Plasma Using Multivariate Model Update Chemometric Methods. 多变量模型更新化学计量学方法测定加标人血浆中吉西他滨和索拉非尼的含量。
IF 1.6 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-11-02 DOI: 10.1093/jaoacint/qsad062
Marco M Z Sharkawi, Norhan R Mohamed, Mohammed T El-Saadi, Noha H Amin

Background: Gemcitabine (GEM), a pyrimidine nucleoside, has been used as a first-line treatment in non-small-cell lung cancer (NSCLC). Sorafenib (SOR), a nonselective multi-kinase inhibitor, is used as a chemotherapeutic agent in different types of cancers including NSCLC in preclinical studies. Co-administration of GEM and SOR was found to be effective and well-tolerated in the treatment of NSCLC.

Objective: The aim of the present work is to determine the studied drugs in spiked human plasma simultaneously through resolving the overlapping spectra and removing the interference of the plasma matrix.

Method: Two updated chemometric models were developed using UV absorbance of the drugs, which named principal component regression (PCR) and partial least-squares (PLS) for determination of GEM and SOR in the ranges of 5-25 and 2-22 µg/mL, respectively.

Results: Validation of the two updated models has been achieved in accordance with US Food and Drug Administration (FDA) guidelines, and the results were satisfactory. The two methods had the advantages of high predictive ability of the studied drugs with high precision and accuracy. Moreover, there was no significant difference obtained when statistical comparison was done between the developed and reported methods, showing good validity of the suggested methods.

Conclusions: The two updated models have the advantages of being rapid, accurate, sensitive, and cost-effective for the determination of GEM and SOR in quality control laboratories without any need for initial separation procedures.

Highlights: Two updated chemometric methods, PCR and PLS, were developed for the estimation of GEM and SOR in spiked human plasma using their UV absorbance data.

背景:吉西他滨(GEM)是一种嘧啶核苷,已被用作非小细胞肺癌(NSCLC)的一线治疗。索拉非尼(SOR)是一种非选择性多激酶抑制剂,在临床前研究中被用作不同类型癌症的化疗药物,包括NSCLC。GEM和SOR联合给药治疗NSCLC有效且耐受性良好。目的:本工作旨在通过消除重叠光谱和消除血浆基质的干扰,同时测定加标人血浆中的研究药物。方法:利用药物的紫外吸光度建立两个更新的化学计量模型,分别命名为主成分回归(PCR)和偏最小二乘(PLS),用于测定5-25和2-22范围内的GEM和SOR µg/mL。结果:两个更新模型的验证符合美国食品药品监督管理局(FDA)的指导方针,结果令人满意。这两种方法具有所研究药物预测能力高、精密度和准确度高的优点。此外,当对所开发的方法和所报道的方法进行统计比较时,没有获得显著差异,表明所建议的方法具有良好的有效性。结论:这两个更新的模型具有快速、准确、灵敏和成本效益高的优点,可在质量控制实验室中测定GEM和SOR,而无需任何初始分离程序。亮点:开发了两种更新的化学计量方法,即PCR和PLS,用于使用其紫外线吸收数据估计加标人血浆中的GEM和SOR。
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引用次数: 0
Efficacy Comparison of an Automated Growth-Based System and Plate-Count Method on the Detection of Yeasts and Molds in Personal Care Products. 基于自动生长的系统和平板计数法检测个人护理产品中酵母菌和霉菌的效果比较。
IF 1.6 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-11-02 DOI: 10.1093/jaoacint/qsad075
Harold A Prada-Ramírez, Sandra Celeita, Juan Camilo Fonseca

Objective: The present investigation studies the efficacy of an automated growth-based system for a quantitative determination of Candida albicans and Aspergillus brasiliensis in several personal care products. The main purpose of this validation study was to prove that the alternative method's entire performance is not inferior to the conventional pour-plate method for a quantitative determination of yeasts and molds. Thus, a performance equivalence was established in accordance with the United Stated Pharmacopeia (USP-NF) Validation of Alternative Microbiological Methods ˂1223˃.

Methods: C. albicans and A. brasiliensis were pooled to use as inoculum (equivalent to 1.0 × 108 CFU/mL) in the suitability of the method test. PCP's preservatives were chemically neutralized leading to the yeast and mold recovery by means of the alternative microbiological method (AMM) and the pour-plate method. A correlation curve was generated for each PCP by plotting DTs relative to the corresponding log CFU values.

Results: Thirty PCPs have been tested for quantification of yeasts and molds using an AMM. An equivalence of results was made through the construction of correlation curves that allowed the establishment of numerically equivalent results between the enumeration data from the reference method (CFU) and the alternative method (Detection times, DTs). Thus, following the guidelines of USP Ch.1223, essential validation parameters were tested, such as equivalence of results (Correlation coeficient, CC >0.95), linearity (R2 >0.9025), accuracy (% recovery >70%), operating range, precision (CV <35%), ruggedness (one-way ANOVA, P > 0.05), specificity, LOD, and LOQ.

Conclusion: It was shown that all the test results obtained from the alternative method were in statistical agreement with the standard plate-count method (PCM). Thus, this new technology was found to meet all the validation criteria needed to be considered for an alternative method for yeast and mold quantification in the PCPs tested.

Highlights: In accordance with the United Stated Pharmacopeia (USP-NF) Validation of Alternative Microbiological Methods ˂1223˃, the implementation of alternative methods can offer benefits in execution and automation while improving accuracy, sensitivity, and precision and reduce the microbiological process time compared to the traditional ones.

目的:研究基于自动生长的系统对几种个人护理产品中白色念珠菌和巴西曲霉的定量测定效果。本验证研究的主要目的是证明替代方法在酵母和霉菌的定量测定中的整体性能不劣于传统的倒板法。因此,根据美国药典(USP-NF)《替代微生物方法验证》1223建立了性能等效性。方法:在方法测试的适用性中,将白色念珠菌和巴西白念珠菌合并用作接种物(相当于1.0×108CFU/mL)。通过替代微生物法(AMM)和倒板法对PCP的防腐剂进行化学中和,从而回收酵母和霉菌。通过绘制相对于相应对数CFU值的DT,为每个PCP生成相关曲线。结果:使用AMM对30个PCP进行了酵母和霉菌的定量测试。通过构建相关曲线,可以在参考方法(CFU)和替代方法(检测时间,DT)的枚举数据之间建立数值等效结果,从而实现结果的等效。因此,根据USP Ch.1223的指南,对基本验证参数进行了测试,如结果等效性(相关系数,CC>0.95)、线性度(R2>0.9025)、准确度(%回收率>70%)、操作范围、精密度(CV 0.05)、特异性、LOD和LOQ。因此,发现这项新技术符合所测试PCP中酵母和霉菌定量替代方法所需的所有验证标准。亮点:根据美国药典(USP-NF)《替代微生物方法验证》1223,与传统方法相比,替代方法的实施可以在执行和自动化方面带来好处,同时提高准确性、敏感性和精密度,并缩短微生物处理时间。
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引用次数: 0
Identification of Radix Bupleuri From Different Geographic Origins Using Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry and Support Vector Machine Algorithm. 基于矩阵辅助激光解吸/电离飞行时间质谱和支持向量机算法鉴定不同地理产地柴胡
IF 1.6 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-11-02 DOI: 10.1093/jaoacint/qsad060
Zheng-Yong Zhang, Ya-Ju Zhao, Fang-Jie Guo, Hai-Yan Wang

Background: The geographic origin of Radix bupleuri is an important factor affecting its efficacy, which needs to be effectively identified.

Objective: The goal is to enrich and develop the intelligent recognition technology applicable to the identification of the origin of traditional Chinese medicine.

Method: This article establishes an identification method of Radix bupleuri geographic origin based on matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) and support vector machine (SVM) algorithm. The Euclidean distance method is used to measure the similarity between Radix bupleuri samples, and the quality control chart method is applied to quantitatively describe their quality fluctuation.

Results: It is found that the samples from the same origin are relatively similar and mainly fluctuate within the control limit, but the fluctuation range is large, and it is impossible to distinguish the samples from different origins. The SVM algorithm can effectively eliminate the impact of intensity fluctuations and huge data dimensions by combining the normalization of MALDI-TOF MS data and the dimensionality reduction of principal components, and finally achieve efficient identification of the origin of Radix bupleuri, with an average recognition rate of 98.5%.

Conclusions: This newly established approach for identification of the geographic origin of Radix bupleuri has been realized, and it has the advantages of objectivity and intelligence, which can be used as a reference for other medical and food-related research.

Highlights: A new intelligent recognition method of medicinal material origin based on MALDI-TOF MS and SVM has been established.

背景:柴胡的地理来源是影响其药效的重要因素,需要进行有效的鉴别。目的:丰富和发展适用于中药产地识别的智能识别技术。方法:建立了一种基于基质辅助激光解吸电离飞行时间质谱(MALDI-TOF MS)和支持向量机(SVM)算法的柴胡产地鉴别方法。采用欧几里得距离法测量柴胡样品之间的相似性,采用质量控制图法定量描述其质量波动。结果:发现同一来源的样品相对相似,主要在控制范围内波动,但波动幅度较大,无法区分不同来源的样品。SVM算法将MALDI-TOF MS数据的归一化与主成分的降维相结合,可以有效地消除强度波动和巨大数据维度的影响,最终实现对柴胡产地的有效识别,平均识别率为98.5%。结论:该新建立的柴胡地理产地识别方法已实现,具有客观性和智能性的优点,可为其他医学和食品相关研究提供参考。亮点:建立了一种新的基于MALDI-TOF MS和SVM的药材产地智能识别方法。
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引用次数: 0
Principles of White Analytical Chemistry and Design of Experiments to Development of Stability-Indicating Chromatographic Method for the Simultaneous Estimation of Thiocolchicoside and Lornoxicam. 白色分析化学原理及稳定性指示色谱法同时测定硫代秋糖苷和氯诺昔康的实验设计。
IF 1.6 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-11-02 DOI: 10.1093/jaoacint/qsad082
Pintu Prajapati, Veera Shakar Pulusu, Shailesh Shah

Background: A variety of chromatographic methods have been published for the stability evaluation of thiocolchicoside (THC) and lornoxicam (LNX). Nevertheless, the development of chromatographic methods requires the use of neurotoxic and teratogenic organic solvents that are detrimental to the environment and harmful to human life.

Objectives: Using the principles of design of experiments (DoE), a novel white analytical chemistry-driven stability-indicating high-performance thin-layer chromatographic (SI-HPTLC) method has been developed for the concurrent stability study of THC and LNX. To protect the environment and human life, the stability-indicating HPTLC method was developed using safe organic solvents.

Method: Potential analytical method risk parameters (AMRPs) and analytical method performance attributes (AMPAs) were screened using the fractional factorial design. The response surface analysis and optimization of critical AMRPs and AMPAs was carried out using full factorial design. Navigation of the method operable design region (MODR) was used to develop the SI-HPTLC technique. The developed method was validated in accordance with the International Council for Harmonization (ICH) Q2 (R1) guideline.

Results: The developed method's greenness was evaluated using the AGREE (Analytical Procedure Greenness) tool and ESA (Eco-Scale Assessment). The Blue (B) model was used to assess the proposed method's cost and time efficiency and user-friendliness. For the stability studies of THC and LNX, the 12 principles of WAC (white analytical chemistry) were used to evaluate the published and proposed chromatographic techniques.

Conclusions: Compared to previously published chromatographic techniques for studying the stability of THC and LNX, the suggested approach was found to be more affordable, environmentally friendly, and user-friendly.

Highlights: The development of a stability-indicating HPTLC method using a novel white analytical chemistry approach and organic solvents with low toxicity potential. Application of the developed method for analysis of the forced degraded sample and fixed-dose combinations of THC and LNX.

背景:已经发表了多种色谱方法来评价硫代秋水仙碱(THC)和氯诺昔康(LNX)的稳定性。然而,色谱法的发展需要使用对环境有害、对人类生命有害的神经毒性和致畸性有机溶剂。目的:利用实验设计原理(DoE),开发了一种新的白色分析化学驱动的稳定性指示高效薄层色谱法(SI-HPTLC),用于THC和LNX的同时稳定性研究。为了保护环境和人类生命安全,采用安全的有机溶剂建立了稳定性指示HPTLC法。方法:采用部分析因设计筛选潜在分析方法风险参数(AMRP)和分析方法性能属性(AMPA)。采用全因子设计对关键AMRP和AMPA进行响应面分析和优化。方法可操作设计区域导航(MODR)用于开发SI-HPTLC技术。根据国际协调理事会(ICH)Q2(R1)指南对所开发的方法进行了验证。结果:使用AGREE(分析程序绿色度)工具和ESA(生态量表评估)对所开发的方法的绿色度进行了评估。Blue(B)模型用于评估所提出的方法的成本和时间效率以及用户友好性。对于THC和LNX的稳定性研究,使用WAC(白色分析化学)的12个原理来评估已发表和提出的色谱技术。结论:与先前发表的用于研究四氢大麻酚和LNX稳定性的色谱技术相比,所提出的方法被发现更经济、环保和用户友好。亮点:使用新型白色分析化学方法和低毒性有机溶剂开发了一种稳定性指示HPTLC方法。所开发的方法在分析强制降解样品和THC和LNX固定剂量组合中的应用。
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引用次数: 0
Quantitative Determination of Organophosphorus, Pyrethroid, and Dithiolane Pesticide Residues in Brown Rice Using Supercritical Fluid Extraction and Liquid Chromatography-Tandem Mass Spectrometry. 超临界萃取-液相色谱-串联质谱法定量测定糙米中有机磷、拟除虫菊酯和二硫代烷农药残留。
IF 1.6 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-11-02 DOI: 10.1093/jaoacint/qsad080
Keisuke Nakamura, Takamitsu Otake, Nobuyasu Hanari

Background: Supercritical fluid extraction (SFE) is a fast, versatile, and solvent-efficient automatic extraction method. Despite its advantages, the results of our proficiency tests imply that the applicability assessments of SFE for pesticide residues were insufficient.

Objective: In this study, as analytical method using SFE was optimized and validated by testing the incurred and fortified brown rice samples with organophosphorus (OP), pyrethroid (PYR), and dithiolane (DIT) pesticides.

Method: A validation study using the incurred sample with etofenprox, fenitrothion, and isoprothiolane was performed by comparing the analytical results obtained using the SFE and solid-liquid extraction with homogenization (SLE), which is a well-validated official multi-residue extraction method. The tests on the fortified samples were also performed for seven pesticide residues, chlorpyrifos, diazinon, O-ethyl O-4-nitrophenyl phenylphosphonothioate (EPN), etofenprox, fenitrothion, isoxathion, and isoprothiolane, at three fortification levels, 0.001, 0.01, and 0.1 mg/kg.

Results: In the test on the incurred samples, optimized SFE-to-SLE analytical values (CSFE/CSLE) were 99.2-100.1%, with RSD lower than 3%. In contrast, the analytical-to-spiked concentrations in the tests on the fortified samples were 96.4-105.0%, with RSD lower than 8.8%.

Conclusions: These results indicate that the proposed SFE method, which is well validated with the incurred brown rice sample, is useful for determining OP, PYR, and DIT pesticide residues in brown rice.

Highlights: The proposed SFE method satisfies EU and Japanese maximum residue limits (MRLs). The consumption of solvent can be reduced to one-fourth of that of SLE using the proposed SFE method.

背景:超临界流体萃取是一种快速、通用、溶剂高效的自动萃取方法。尽管SFE具有优势,但我们的能力测试结果表明,SFE对农药残留的适用性评估不足。目的:本研究通过对含有有机磷(OP)、拟除虫菊酯类(PYR)和二硫杂环戊烯(DIT)农药的糙米样品进行检测,优化并验证了SFE的分析方法。方法:通过比较SFE和固液提取均化法(SLE)获得的分析结果,使用埃托芬prox、杀硝基苯和异硫平产生的样品进行验证研究,这是一种经过充分验证的官方多残留提取方法。在三个强化水平(0.001、0.01和0.1)下,还对强化样品进行了7种农药残留的测试,即毒死蜱、二嗪农、O-乙基-4-硝基苯基硫代膦酸酯(EPN mg/kg。结果:在对所产生样品的测试中,SFE对SLE的最佳分析值(CSFE/CSLE)为99.2-100.1%,RSD低于3%。与此相反,强化样品的分析加标浓度为96.4-105.0%,RSD低于8.8%。结论:该方法可用于糙米中OP、PYR和DIT农药残留的测定。亮点:拟议的SFE方法符合欧盟和日本的最大残留限量。使用所提出的SFE方法,溶剂的消耗可以减少到SLE的四分之一。
{"title":"Quantitative Determination of Organophosphorus, Pyrethroid, and Dithiolane Pesticide Residues in Brown Rice Using Supercritical Fluid Extraction and Liquid Chromatography-Tandem Mass Spectrometry.","authors":"Keisuke Nakamura,&nbsp;Takamitsu Otake,&nbsp;Nobuyasu Hanari","doi":"10.1093/jaoacint/qsad080","DOIUrl":"10.1093/jaoacint/qsad080","url":null,"abstract":"<p><strong>Background: </strong>Supercritical fluid extraction (SFE) is a fast, versatile, and solvent-efficient automatic extraction method. Despite its advantages, the results of our proficiency tests imply that the applicability assessments of SFE for pesticide residues were insufficient.</p><p><strong>Objective: </strong>In this study, as analytical method using SFE was optimized and validated by testing the incurred and fortified brown rice samples with organophosphorus (OP), pyrethroid (PYR), and dithiolane (DIT) pesticides.</p><p><strong>Method: </strong>A validation study using the incurred sample with etofenprox, fenitrothion, and isoprothiolane was performed by comparing the analytical results obtained using the SFE and solid-liquid extraction with homogenization (SLE), which is a well-validated official multi-residue extraction method. The tests on the fortified samples were also performed for seven pesticide residues, chlorpyrifos, diazinon, O-ethyl O-4-nitrophenyl phenylphosphonothioate (EPN), etofenprox, fenitrothion, isoxathion, and isoprothiolane, at three fortification levels, 0.001, 0.01, and 0.1 mg/kg.</p><p><strong>Results: </strong>In the test on the incurred samples, optimized SFE-to-SLE analytical values (CSFE/CSLE) were 99.2-100.1%, with RSD lower than 3%. In contrast, the analytical-to-spiked concentrations in the tests on the fortified samples were 96.4-105.0%, with RSD lower than 8.8%.</p><p><strong>Conclusions: </strong>These results indicate that the proposed SFE method, which is well validated with the incurred brown rice sample, is useful for determining OP, PYR, and DIT pesticide residues in brown rice.</p><p><strong>Highlights: </strong>The proposed SFE method satisfies EU and Japanese maximum residue limits (MRLs). The consumption of solvent can be reduced to one-fourth of that of SLE using the proposed SFE method.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"1532-1541"},"PeriodicalIF":1.6,"publicationDate":"2023-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9829640","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}
引用次数: 0
Validation of the KangarooSci® Aerobic Count Plate for the Enumeration of Meosphilic Aerobic Bacteria in Selected Foods and on Stainless Steel Environmental Surfaces: AOAC Performance Tested MethodSM 062301. KangarooSci®好氧计数板在选定食品和不锈钢环境表面中嗜氧需氧细菌计数的验证:AOAC性能测试方法sm 062301。
IF 1.6 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-11-02 DOI: 10.1093/jaoacint/qsad088
Danping Wei, Di Wu, Jisheng Wang, Yazhou Li, Xinyu Sun, Can Zhang, Shuai Zhang, Wesley Thompson, M Joseph Benzinger, Erin Crowley

Background: The KangarooSci® Aerobic Count Plate (ACP) is a sample-ready culture medium system for direct counting of aerobic bacteria colonies after 48-72 h of incubation.

Objective: The KangarooSci ACP was evaluated for AOAC Performance Tested MethodsSM certification.

Methods: The KangarooSci ACP was evaluated through matrix studies and product consistency/stability study and robustness testing. For the matrix study, nine food products (nonfat dry milk powder, fresh raw bovine milk, pasteurized liquid bovine milk, fresh raw ground beef, frozen uncooked chicken breast, cooked shredded pork, apple juice, ice cream, and fresh strawberries), and one environmental surface (stainless steel) were evaluated following the KangarooSci ACP product instructions and compared to the ISO 4833-1:2013, Microbiology of food and animal feeding stuffs-Horizontal methods for the enumeration of microorganisms-Part 1: Colony count at 30 °C by the pour plate technique reference standard. The product consistency and stability testing evaluated three separate production lots of the KangarooSci ACP. The robustness testing examined three test parameters, volume of sample plated, incubation time, and incubation temperature, using a factorial study design.

Results: Results from the matrix study demonstrated equivalent performance between the KangarooSci ACP and the ISO 4833-1:2013 reference standard. The product consistency and stability testing showed that the performance of the assay was equivalent over time up to 12 months and between production lots. Minor changes to the operational test conditions showed no significant impact on performance during the robustness testing.

Conclusion: The KangarooSci ACP is an effective method for aerobic plate count for all matrixes evaluated.

Highlights: The KangarooSci ACP allows for fast, reliable enumeration of aerobic bacteria. Utilizing the alternative method takes up less space in incubators, requires no sample spreader, and requires fewer consumables compared to the reference method.

背景:KangaroSci®需氧菌计数板(ACP)是一种可直接计数48-72后需氧菌菌落的样品培养基系统 孵育h。目的:对KangaroSci-ACP进行AOAC性能测试方法SM认证。方法:通过基质研究、产品一致性/稳定性研究和稳健性测试对KangaroSci-ACP进行评估。在基质研究中,九种食品(脱脂奶粉、新鲜生牛乳、巴氏灭菌液态牛乳、新鲜生碎牛肉、冷冻生鸡胸肉、熟肉丝、苹果汁、冰淇淋和新鲜草莓)和一种环境表面(不锈钢)按照KangaroSci-ACP产品说明进行了评估,并与ISO 4833-1:2013进行了比较,食品和动物饲料的微生物学微生物计数的水平方法第1部分:30时的菌落计数 °C,采用浇注板技术参考标准。产品一致性和稳定性测试评估了KangaroSci-ACP的三个独立生产批次。稳健性测试使用析因研究设计检查了三个测试参数,即样品电镀体积、培养时间和培养温度。结果:基质研究的结果表明,KangaroSci-ACP和ISO 4833-1:2013参考标准的性能相当。产品一致性和稳定性测试表明,在长达12 月和生产批次之间。在稳健性测试期间,操作测试条件的微小变化对性能没有显著影响。结论:KangaroSci-ACP是一种对所有基质进行有氧平板计数的有效方法。亮点:袋鼠科学ACP允许快速、可靠地计数需氧细菌。与参考方法相比,使用替代方法在培养箱中占用更少的空间,不需要样品散布器,并且需要更少的耗材。
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引用次数: 0
A Review on Analytical Methods for Tigecycline Estimation From Its Bulk and Dosage Form. 替加环素原料药和剂型分析方法综述。
IF 1.6 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-11-02 DOI: 10.1093/jaoacint/qsad099
Bansi Rakholiya, Priyangi Shah, Yash Patel, Gayatri Patel, Samir Patel, Archita Patel

Background: Tigecycline (TIG) is a third-generation glycylcycline derivative used as an antimicrobial and anticancer agent for the past few years. Its intricate structure makes it more vulnerable toward degradation under the influence of various environmental factors and leads to the generation of impurities. Due to its stability issues, TIG is available as a lyophilized powder for injection. The analysis of TIG becomes a cumbersome task for analysts due to its instability in solution form. As TIG works as a life-saving drug, it is important to review its analytical methods for its quality control.

Objective: The present review discusses various analytical methodologies for determining TIG from its bulk, lyophilized powder, pharmacopoeial methods and factors responsible for its instability.

Methods: The present review represents the analysis of data reported in the literature from 1999-2022 for the analysis of TIG.

Results: Numerous alternative analytical techniques such as UV-visible spectrophotometry, spectrofluorimetric methods, RP-HPLC (reversed-phase high-performance liquid chromatography) and FT-IR (Fourier transform infrared), and electrophoresis has been reported for quantification, identification, and characterization of TIG.

Conclusions: Several analytical techniques are available to be used as a quality control tool for tigecycline, including HPLC without derivatization, whereas the fluorescence technique requires derivatization using acidic dye. A few methods require tedious pre-sample preparation techniques, become time-consuming, and involve using one or more organic solvents; there is a need to develop eco-friendlier methods for analyzing tigecycline.

Highlights: Various analytical methods such as spectrometric, fluorimetric and chromatographic methods have been discussed for estimation of TIG from its bulk and different dosage form.

背景:替加环素(TIG)是近几年来作为抗微生物和抗癌药物使用的第三代甘氨酰环素衍生物。其复杂的结构使其在各种环境因素的影响下更容易降解,并导致杂质的产生。由于其稳定性问题,TIG可用作注射用冻干粉。由于TIG溶液形式的不稳定性,其分析对分析人员来说是一项繁琐的任务。由于TIG是一种救命药物,因此审查其分析方法对其质量控制很重要。目的:从TIG的散装、冻干粉、药典方法和导致其不稳定性的因素等方面讨论了TIG的各种分析方法。方法:对1999-2022年TIG分析文献中的数据进行分析。结果:紫外-可见分光光度法、荧光光谱法、RP-HPLC(反相高效液相色谱法)和FT-IR(傅立叶变换红外法)等多种可供选择的分析技术,和电泳已被报道用于TIG的定量、鉴定和表征。结论:有几种分析技术可用于替加环素的质量控制工具,包括没有衍生化的HPLC,而荧光技术需要使用酸性染料进行衍生化。一些方法需要繁琐的样品前制备技术,变得耗时,并且需要使用一种或多种有机溶剂;需要开发更环保的方法来分析替加环素。亮点:讨论了从TIG的体积和不同剂型估算TIG的各种分析方法,如光谱法、荧光法和色谱法。
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引用次数: 0
Utilization of Chemometric-Aided UV Spectrophotometric Methods for Concurrent Assessment of Emtricitabine, Tenofovir Disoproxil Fumarate, Elvitegravir, and Cobicistat in Tablet Formulation. 化学计量辅助紫外分光光度法同时评价恩曲他滨、富马酸替诺福韦二氧吡酯、依维替韦和可比司他在片剂中的含量。
IF 1.6 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-11-02 DOI: 10.1093/jaoacint/qsad067
Veena D Singh, Vijay K Singh, Sanjay J Daharwal

Background: Emtricitabine (ETC), tenofovir disoproxil fumarate (TNF), elvitegravir (EVG), and cobicistat (CBS) are antiviral drugs used to treat human immunodeficiency virus (HIV) infections.

Objective: To develop chemometric-aided UV spectrophotometric methods for concurrent estimation of the aforementioned drugs used to treat HIV. This method can be used to reduce modification of the calibration model by assessing the absorbance at various points in the zero-order spectra within the selected wavelength range. Additionally, it eliminates interfering signals and provides sufficient resolution in multi-component systems.

Methods: Two chemometric-assisted UV spectrophotometric methods, namely, partial least-squares (PLS) and principal component regression (PCR) models, were established for the concurrent assessment of EVG, CBS, TNF, and ETC in tablet formulations. The proposed methods were applied to decrease complexity of overlapped spectra and to achieve maximum sensitivity and the lowest error. These approaches were performed in accordance with International Council on Harmonization (ICH) criteria and compared to the reported HPLC method.

Results: The proposed methods were used to assess EVG, CBS, TNF, and ETC in the ranges of 5-30, 5-30 , 5-50, and 5-50 µg/mL, respectively, with an excellent correlation coefficient (r2 ≥ 0.998). The accuracy and precision results were found to be within the acceptable limits. No statistical difference was observed between the proposed and reported studies.

Conclusion: The chemometric-aided UV spectrophotometric approaches could be considered as alternatives to chromatographic procedures in the pharmaceutical industry for routine analysis and testing of readily accessible commercial formulations.

Highlights: Novel chemometric-assisted UV spectrophotometric techniques were developed for assessment of multicomponent antiviral combinations in single-tablet formulations. The proposed methods were performed without using harmful solvents, tedious preparation, or expensive instruments. The proposed methods were compared statistically with a reported HPLC method. Assessment of EVG, CBS, TNF, and ETC was performed without interference from excipients in their multicomponent formulations.

背景:恩曲他滨(ETC)、富马酸替诺福韦二酯(TNF)、依韦替拉韦(EVG)和钴司他(CBS)是用于治疗人类免疫缺陷病毒(HIV)感染的抗病毒药物。目的:建立化学计量辅助紫外分光光度法同时测定上述治疗HIV药物的方法。该方法可用于通过评估所选波长范围内零阶光谱中各个点的吸光度来减少校准模型的修改。此外,它消除了干扰信号,并在多分量系统中提供了足够的分辨率。方法:建立两种化学计量辅助紫外分光光度法,即偏最小二乘(PLS)和主成分回归(PCR)模型,用于同时评估片剂配方中的EVG、CBS、TNF和ETC。将所提出的方法应用于降低重叠谱的复杂度,实现最大的灵敏度和最小的误差。这些方法是根据国际协调理事会(ICH)标准进行的,并与报道的HPLC方法进行了比较。结果:所提出的方法用于评估EVG、CBS、TNF和ETC,范围为5-30、5-30 , 5-50和5-50 µg/mL,具有良好的相关系数(r2 ≥ 0.998)。准确度和精密度结果在可接受的限度内。建议的研究和报告的研究之间没有观察到统计学差异。结论:化学计量辅助紫外分光光度法可作为制药行业色谱程序的替代品,用于对易于获得的商业制剂进行常规分析和测试。亮点:开发了新的化学计量辅助紫外分光光度法技术,用于评估单片制剂中的多组分抗病毒组合。所提出的方法在不使用有害溶剂、繁琐的制备或昂贵的仪器的情况下进行。将所提出的方法与已报道的HPLC方法进行统计学比较。EVG、CBS、TNF和ETC的评估在其多组分制剂中不受赋形剂干扰的情况下进行。
{"title":"Utilization of Chemometric-Aided UV Spectrophotometric Methods for Concurrent Assessment of Emtricitabine, Tenofovir Disoproxil Fumarate, Elvitegravir, and Cobicistat in Tablet Formulation.","authors":"Veena D Singh,&nbsp;Vijay K Singh,&nbsp;Sanjay J Daharwal","doi":"10.1093/jaoacint/qsad067","DOIUrl":"10.1093/jaoacint/qsad067","url":null,"abstract":"<p><strong>Background: </strong>Emtricitabine (ETC), tenofovir disoproxil fumarate (TNF), elvitegravir (EVG), and cobicistat (CBS) are antiviral drugs used to treat human immunodeficiency virus (HIV) infections.</p><p><strong>Objective: </strong>To develop chemometric-aided UV spectrophotometric methods for concurrent estimation of the aforementioned drugs used to treat HIV. This method can be used to reduce modification of the calibration model by assessing the absorbance at various points in the zero-order spectra within the selected wavelength range. Additionally, it eliminates interfering signals and provides sufficient resolution in multi-component systems.</p><p><strong>Methods: </strong>Two chemometric-assisted UV spectrophotometric methods, namely, partial least-squares (PLS) and principal component regression (PCR) models, were established for the concurrent assessment of EVG, CBS, TNF, and ETC in tablet formulations. The proposed methods were applied to decrease complexity of overlapped spectra and to achieve maximum sensitivity and the lowest error. These approaches were performed in accordance with International Council on Harmonization (ICH) criteria and compared to the reported HPLC method.</p><p><strong>Results: </strong>The proposed methods were used to assess EVG, CBS, TNF, and ETC in the ranges of 5-30, 5-30 , 5-50, and 5-50 µg/mL, respectively, with an excellent correlation coefficient (r2 ≥ 0.998). The accuracy and precision results were found to be within the acceptable limits. No statistical difference was observed between the proposed and reported studies.</p><p><strong>Conclusion: </strong>The chemometric-aided UV spectrophotometric approaches could be considered as alternatives to chromatographic procedures in the pharmaceutical industry for routine analysis and testing of readily accessible commercial formulations.</p><p><strong>Highlights: </strong>Novel chemometric-assisted UV spectrophotometric techniques were developed for assessment of multicomponent antiviral combinations in single-tablet formulations. The proposed methods were performed without using harmful solvents, tedious preparation, or expensive instruments. The proposed methods were compared statistically with a reported HPLC method. Assessment of EVG, CBS, TNF, and ETC was performed without interference from excipients in their multicomponent formulations.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":" ","pages":"1673-1681"},"PeriodicalIF":1.6,"publicationDate":"2023-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"9586789","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}
引用次数: 0
Eco-Friendly UV-Spectrophotometric Methods Employing Magnetic Nano-Composite Polymer for the Extraction and Analysis of Sexual Boosters in Adulterated Food Products: Application of Computer-Aided Design. 磁性纳米复合聚合物紫外分光光度法提取分析掺假食品中的性促进剂:计算机辅助设计的应用
IF 1.6 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-11-02 DOI: 10.1093/jaoacint/qsad084
Mohamed A Abdelshakour, Khaled Attala, Ahmed Elsonbaty, Randa A Abdel Salam, Ghada M Hadad, Aziza E Mostafa, Maya S Eissa

Background: Solid phase extraction (SPE) techniques, based on computationally designed magnetic-based multi-targeting molecular imprinted polymer (MT-MIP), combined with UV spectrophotometric approaches provide advantages in the examination of counterfeit samples.

Objective: The current work describes an innovative and sustainable methodology for the simultaneous determination of tadalafil (TAD) and dapoxetine hydrochloride (DAP) in aphrodisiac counterfeit products (honey and instant coffee) utilizing SPE exploiting MT-MIP. Additionally, an innovative UV spectrophotometric method capable of resolving TAD in its pharmaceutical binary mixtures with DAP was developed. A novel computational approach was implemented to tailor the synthesis and design of the MT-MIP particles.

Methods: We applied a newly developed UV spectrophotometric method which was based on a Fourier self-deconvolution (FSD) method coupled with the isoabsorptive point for determination of TAD and DAP in pharmaceutical dosage form. We also applied an SPE process based on MT-MIP designed particles, assisting in the analysis of both drugs in counterfeit food samples. The SPE process and the UV spectroscopic methodology were assessed regarding their greenness using the pioneering green analytical procedure index (GAPI), analytical greeness including sample preparation (AGREEprep) and AGREE tools. The synthesized MT-MIP particles were characterized by scanning electron microscopy and energy-dispersive x-ray spectroscopy.

Results: The suggested spectrophotometric methods revealed a wide linear concentration range of 2-50 µg/mL with lower LODs in the range of 0.604-0.994 µg/mL. Additionally, the suggested method demonstrated the utmost sensitivity and eco-friendliness for their target in its mixed dosage form and counterfeit food products.

Conclusion: The SPE process and the developed analytical UV spectroscopic methodology were validated as per the ICH guidelines, and were found to be suitable for overseeing some counterfeiting activities in commercially available honey and instant coffee aphrodisiac products.

Highlights: An SPE method based on MT-MIP magnetic-based polymer and a UV spectroscopic method were successfully developed for analysis of TAD and DAP in different matrices.

背景:固相萃取(SPE)技术基于计算设计的磁性多靶向分子印迹聚合物(MT-MIP),结合紫外分光光度法,在检测假冒样品方面具有优势。目的:本工作描述了一种创新和可持续的方法,利用SPE利用MT-MIP同时测定壮阳假冒产品(蜂蜜和速溶咖啡)中的他达拉非(TAD)和盐酸达泊西汀(DAP)。此外,还开发了一种创新的紫外分光光度法,能够用DAP分离药物二元混合物中的TAD。实现了一种新的计算方法来定制MT-MIP粒子的合成和设计。方法:采用一种新开发的基于傅立叶自去卷积(FSD)法和等吸收点的紫外分光光度法测定药物剂型中的TAD和DAP。使用开创性的绿色分析程序指数(GAPI)、包括样品制备在内的分析绿色性(AGREEprep)和AGREE工具,对SPE工艺和UV光谱方法的绿色性进行了评估。用扫描电子显微镜和能谱仪对合成的MT-MIP颗粒进行了表征。结果:建议的分光光度法显示出2-50的宽线性浓度范围 µg/mL,LOD较低,范围为0.604-0.994 µg/mL。此外,所提出的方法对其混合剂型和假冒食品中的目标表现出最大的敏感性和生态友好性。结论:SPE工艺和所开发的紫外光谱分析方法已根据ICH指南进行了验证,并被发现适用于监督商业蜂蜜和速溶咖啡壮阳产品中的一些假冒活动。亮点:成功开发了一种基于MT-MIP磁性聚合物的SPE方法和一种紫外光谱方法,用于分析不同基质中的TAD和DAP。
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引用次数: 1
Consumer-Led Investigation into Potential Issues That Arise When Testing Dairy Matrixes for Gluten With the NIMA Sensor. 消费者主导的调查在使用NIMA传感器检测谷蛋白乳制品基质时出现的潜在问题。
IF 1.6 4区 农林科学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2023-11-02 DOI: 10.1093/jaoacint/qsad092
Tricia Thompson, Adrian Rogers, Johnna Perry

Background: Some consumers with celiac disease use personal, point-of-use gluten detection devices to test food. False-positive results may occur due to sampling, matrix effects, and sensor issues.

Objective: The purpose of the present study was to determine if the positive gluten results some users were obtaining when testing cream cheese and materials of similar consistency were false positives and, if so, what might be causing them to occur.

Methods: Cream cheese, soft cheese, and yogurt were tested for gluten using the Ridascreen Gliadin R7001 sandwich R5 ELISA and the Ridascreen Gliadin R7021 competitive R5 ELISA. Two test portions were taken, extracted, and tested from each homogenized material. Materials were also analyzed for gluten using a NIMA sensor, a personal, point-of-use gluten detection device. Multiple test portion weights were tested beginning at 0.13 to 0.17 g (the ideal weight of the test portion according to the NIMA sensor development team).

Results: Using the sandwich R5 ELISA and the competitive R5 ELISA, all materials tested below the lower LOD for gluten. Using a NIMA sensor, as the weight of the test portion tested increased, sensor results went from no gluten found, to gluten found, to no test result.

Conclusion: The gluten found results using the NIMA sensor are likely false positives that appear to correspond with the weight and volume of the material tested, as well as the viscosity. There is also an apparent disconnect between the gluten found result reported by the sensor and an interpretation of the lateral flow device (LFD) strip result when assessed by eye which should also be taken into account. Ideally, NIMA sensor users should be advised on the weight amount of material to analyze and test portions should be weighed before being used with the NIMA sensor. However, this is not a practical solution when testing in many environments, including restaurants.

Highlights: Slight variations in weight and volume of test materials can result in false positive results when testing dairy matrixes for gluten using the Nima sensor.

背景:一些患有乳糜泻的消费者使用个人的、即用即用的谷蛋白检测设备来检测食物。由于采样、矩阵效应和传感器问题,可能会出现假阳性结果。目的:本研究的目的是确定一些用户在测试奶油奶酪和类似稠度的材料时获得的阳性面筋结果是否为假阳性,如果是,是什么原因导致了假阳性。方法:使用Ridascreen Gliadin R7001夹心R5 ELISA和Ridascren GliadinR7021竞争性R5 ELISA检测奶油奶酪、软奶酪和酸奶的面筋。从每种均化材料中取出、提取并测试两个测试部分。还使用NIMA传感器对材料的面筋进行了分析,NIMA传感器是一种个人使用点面筋检测设备。从0.13至0.17克(根据NIMA传感器开发团队的说法,这是测试部分的理想重量)开始测试多个测试部分的重量。结果:使用三明治R5 ELISA和竞争性R5 ELISA,所有材料的测试都低于面筋的较低LOD。使用NIMA传感器,随着测试部分重量的增加,传感器结果从没有发现麸质,到发现麸质再到没有测试结果。结论:使用NIMA传感器发现的面筋结果可能是假阳性,似乎与测试材料的重量和体积以及粘度相对应。传感器报告的面筋发现结果与用眼睛评估时对侧流装置(LFD)条带结果的解释之间也存在明显的脱节,这也应考虑在内。理想情况下,应向NIMA传感器用户建议要分析的材料的重量,并在与NIMA传感器一起使用之前对测试部分进行称重。然而,在包括餐馆在内的许多环境中进行测试时,这并不是一个实用的解决方案。亮点:当使用Nima传感器测试乳制品基质中的面筋时,测试材料的重量和体积的微小变化可能会导致假阳性结果。
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引用次数: 0
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Journal of AOAC International
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