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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 Q2 Medicine 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。
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引用次数: 0
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 Q2 Medicine 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
Validation of an HPLC Method for the Determination of Diclofenac Diethylamine and Three of Its Impurities in a Gel Pharmaceutical Form. 凝胶制剂中双氯芬酸二乙胺及其三种杂质的高效液相色谱测定方法的验证。
IF 1.6 4区 农林科学 Q2 Medicine Pub Date : 2023-11-02 DOI: 10.1093/jaoacint/qsad078
Mounir El Kacemi, Aimen El Orche, Omar Elhamdaoui, Amine Laouni, Mohamed Azougagh, Khalid Karrouchi, Mustapha Bouatia, Miloud El Karbane

Background: Monitoring impurities in drug products is a principal requirement of pharmaceutical regulatory authorities all over the world to ensure drug safety. For this reason, there is a great need for analytical QC of dugs products.

Objective: In this study, a simple, efficient, and direct HPLC method was developed for the determination of three impurities of diclofenac.

Methods: The HPLC method was developed using a mobile phase which consisted of an HPLC grade mixture, acetonitrile-0.01M phosphoric acid adjusted to pH 2.3 (1 + 3, by volume).

Results: The separation was performed in 15 min. The calibration curves of the three impurities were linear; the correlation coefficients were 0.999 at concentrations of 0.00015-0.003 µg/mL.

Conclusion: The validation of this method shows that it meets all validation criteria. This shows the reliability of this method for the routine control of diclofenac impurities.

Highlights: The validation of a robust HPLC method for the determination of diclofenac impurities is of great importance for the pharmaceutical industry to control its products.

背景:监测药品中的杂质是世界各地药品监管部门确保药品安全的主要要求。因此,非常需要对羽绒被产品进行分析质量控制。目的:建立一种简便、高效、直接的高效液相色谱法测定双氯芬酸中三种杂质的含量。方法:采用高效液相色谱法,流动相为乙腈-0.01M磷酸,pH调节至2.3(1+3,按体积计) min.三种杂质的校准曲线为线性;浓度为0.00015-0.003时,相关系数为0.999 µg/mL。结论:该方法的验证表明,它符合所有验证标准。这表明该方法用于双氯芬酸杂质的常规控制是可靠的。亮点:高效液相色谱法测定双氯芬酸杂质的验证对制药行业控制其产品具有重要意义。
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引用次数: 0
Green Method for Evaluation of Marbofloxacin Tablets by HPLC and Evaluation of Interchangeability With UV and Turbidimetric Methods. 高效液相色谱法评价马布沙星片的绿色方法及与紫外和浊度法的互换性评价。
IF 1.6 4区 农林科学 Q2 Medicine Pub Date : 2023-11-02 DOI: 10.1093/jaoacint/qsad102
Aline Sinzervinch de Oliveira, Naiara Raica Lopes de Oliveira, Jerônimo Raimundo de Oliveira Neto, Layla Lopes Tavares, Ana Carolina Kogawa

Background: Marbofloxacin (MAR) is a veterinary antimicrobial, marketed in injectable solution, oral suspension, and tablets. MAR has no monograph for tablet evaluation in official compendiums. High Performance Liquid Chromatography (HPLC) methods present in the literature for evaluating MAR in tablets do not follow the principles of green and sustainable analytical chemistry.

Objective: A green, clean, and sustainable method by HPLC was developed and validated to evaluate the content and stability of MAR in tablets, in addition to comparing it with other methods available in the literature.

Method: A C8, 5 µm, 4.6 × 150 mm (ACE®) column, purified water with 0.2% formic acid-ethanol (70:30, v/v) as the mobile phase, and a flow rate of 0.7 mL/min at 296 nm were used.

Results: The method was linear over a concentration range of 1-10 μg/mL, selective for tablet matrix and forced degradation, precise with relative standard deviations (RDS) less than 5%, accurate with recovery of 99.99%, and robust to changes in the mobile phase, flow rate, wavelength, equipment, and column brand. The retention time for MAR was approximately 3.1 min.

Conclusions: The method can be used in routine analysis of MAR in tablets in chemical-pharmaceutical laboratories. Furthermore, it can be used to verify the stability of MAR-based products and proved to be interchangeable with spectrophotometric method in the UV region and turbidimetric microbiological method.

Highlights: A green method for evaluation of marbofloxacin tablets by HPLC was developed and validated. Additionally, it has been shown to be interchangeable with UV and turbidimetric methods.

背景:马波沙星(MAR)是一种兽医抗菌药物,以注射溶液、口服混悬液和片剂的形式上市。MAR在官方汇编中没有关于片剂评价的专著。文献中用于评估片剂中MAR的高效液相色谱(HPLC)方法不符合绿色和可持续分析化学的原则。目的:建立并验证了一种绿色、清洁、可持续的高效液相色谱法来评价MAR在片剂中的含量和稳定性,并与文献中的其他方法进行了比较。方法:A C8,5 µm,4.6×150 mm(ACE®)柱,流动相为0.2%甲酸乙醇(70:30,v/v)的纯化水,流速为0.7 296时为mL/min nm。结果:该方法在1-10的浓度范围内呈线性 μg/mL,对片剂基质和强制降解具有选择性,精密度相对标准偏差(RDS)小于5%,准确度回收率为99.99%,对流动相、流速、波长、设备和柱品牌的变化具有鲁棒性。MAR的保留时间约为3.1 结论:该方法可用于化学制药实验室片剂中MAR的常规分析。此外,它可用于验证MAR基产品的稳定性,并被证明可与紫外区域的分光光度法和浊度微生物法互换。亮点:建立并验证了高效液相色谱法评价马波沙星片的绿色方法。此外,它已被证明可以与紫外线和浊度法互换。
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引用次数: 0
Assessment of the Water Sorption Capacity of Rifaximin Using the Dynamic Vapor Sorption Technique for Optimization of the Choice of Excipients and the Manufacturing Environment of Rifaximin Tablets. 动态气相吸附法评价利福昔明的吸水性能,优化辅料的选择及利福昔明片的生产环境。
IF 1.6 4区 农林科学 Q2 Medicine Pub Date : 2023-11-02 DOI: 10.1093/jaoacint/qsad103
Naga Venkata Durga Prasad Ketha, Hanimi Reddy Bapatu, Kumara Swami Ummiti, Praveen Kumar Subbappa, Deepti Kolli

Background: Rifaximin, a medication of the rifamycin family with two distinct strengths of 200 mg and 550 mg in tablet form, is useful for the treatment of travelers' diarrhea. It has a solid yellow hue and is very hygroscopic in nature. It exhibits a variety of polymorphic forms such as α, β, γ, δ, and ε depending on bonded moisture. These polymorphs' varying chemical and physical characteristics, such as solubility and water content, may have a big impact on in vivo absorption, which in turn affects efficacy and safety. Therefore, understanding the polymorphic stability of rifaximin is crucial for formulating rifaximin tablets.

Objective: The current effort focuses on the understanding of water vapor sorption properties to control the polymorphic stability of rifaximin in the tablet formulation using the appropriate selection of excipients and manufacturing process.

Methods: The dynamic vapor sorption method in the range of 0-90% relative humidity at 25°C is used for understanding the sorption properties of drug substances and drug excipient mixtures; the state-of-the-art techniques of the X-ray diffraction method are used to identify polymorph conversions; and dissolution procedures are used for in vitro correlation studies.

Results: The sorption study data reveals that rifaximin is highly unstable at relative humidity conditions above 36%. When using excipients that have a low tendency to adsorb water in the formulation, the polymorphic results do not show any change in their intended form, and the in vitro dissolution data show an equivalency with the reference drug product.

Conclusion: The study prompted a successful outcome-oriented development of the formulation processing environment conditions design to develop a test formulation that has adequate polymorphic stability and also similarity in in-vitro dissolution profiles, with the reference product with highest similarity.

Highlights: The overall study described here is useful for swiftly gaining insight into the sorption characteristics of rifaximin, and it contributes to the widespread acceptance of rifaximin tablets as a treatment option.

背景:利福霉素家族的一种药物,具有两种不同的200 mg和550 片剂形式的mg可用于治疗旅行者腹泻。它有一个坚实的黄色色调,是非常吸湿性的性质。根据结合水分的不同,它表现出多种多晶型,如α、β、γ、δ和ε。这些多晶型物不同的化学和物理特性,如溶解度和含水量,可能会对体内吸收产生重大影响,进而影响疗效和安全性。因此,了解利福昔明的多态性稳定性对于配制利福昔敏片剂至关重要。目的:目前的工作重点是了解水蒸气吸附特性,通过适当选择辅料和生产工艺来控制利福昔明在片剂配方中的多态性稳定性。方法:采用25°C相对湿度0-90%范围内的动态气相吸附法,了解原料药和辅料混合物的吸附性能;使用X射线衍射方法的最先进技术来鉴定多晶型转化率;以及溶出程序用于体外相关性研究。结果:吸附研究数据表明,利福昔明在相对湿度超过36%的条件下是高度不稳定的。当使用制剂中吸水性低的赋形剂时,多晶型结果没有显示其预期形式的任何变化,体外溶出度数据显示与参考药物产品相当。结论:该研究促进了以结果为导向的制剂加工环境条件设计的成功开发,以开发一种具有足够多态性稳定性和体外溶出度相似性的试验制剂,与相似性最高的参考产品。亮点:本文所述的整体研究有助于迅速深入了解利福昔明的吸附特性,并有助于利福昔敏片作为一种治疗选择的广泛接受。
{"title":"Assessment of the Water Sorption Capacity of Rifaximin Using the Dynamic Vapor Sorption Technique for Optimization of the Choice of Excipients and the Manufacturing Environment of Rifaximin Tablets.","authors":"Naga Venkata Durga Prasad Ketha,&nbsp;Hanimi Reddy Bapatu,&nbsp;Kumara Swami Ummiti,&nbsp;Praveen Kumar Subbappa,&nbsp;Deepti Kolli","doi":"10.1093/jaoacint/qsad103","DOIUrl":"10.1093/jaoacint/qsad103","url":null,"abstract":"<p><strong>Background: </strong>Rifaximin, a medication of the rifamycin family with two distinct strengths of 200 mg and 550 mg in tablet form, is useful for the treatment of travelers' diarrhea. It has a solid yellow hue and is very hygroscopic in nature. It exhibits a variety of polymorphic forms such as α, β, γ, δ, and ε depending on bonded moisture. These polymorphs' varying chemical and physical characteristics, such as solubility and water content, may have a big impact on in vivo absorption, which in turn affects efficacy and safety. Therefore, understanding the polymorphic stability of rifaximin is crucial for formulating rifaximin tablets.</p><p><strong>Objective: </strong>The current effort focuses on the understanding of water vapor sorption properties to control the polymorphic stability of rifaximin in the tablet formulation using the appropriate selection of excipients and manufacturing process.</p><p><strong>Methods: </strong>The dynamic vapor sorption method in the range of 0-90% relative humidity at 25°C is used for understanding the sorption properties of drug substances and drug excipient mixtures; the state-of-the-art techniques of the X-ray diffraction method are used to identify polymorph conversions; and dissolution procedures are used for in vitro correlation studies.</p><p><strong>Results: </strong>The sorption study data reveals that rifaximin is highly unstable at relative humidity conditions above 36%. When using excipients that have a low tendency to adsorb water in the formulation, the polymorphic results do not show any change in their intended form, and the in vitro dissolution data show an equivalency with the reference drug product.</p><p><strong>Conclusion: </strong>The study prompted a successful outcome-oriented development of the formulation processing environment conditions design to develop a test formulation that has adequate polymorphic stability and also similarity in in-vitro dissolution profiles, with the reference product with highest similarity.</p><p><strong>Highlights: </strong>The overall study described here is useful for swiftly gaining insight into the sorption characteristics of rifaximin, and it contributes to the widespread acceptance of rifaximin tablets as a treatment option.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10180476","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
A New JECFA Method for GC-MS Determination of Propylene Chlorohydrine Residues in Hydroxypropylated Starches. GC-MS法测定羟丙基淀粉中丙二氯丙烷残留量
IF 1.6 4区 农林科学 Q2 Medicine Pub Date : 2023-09-01 DOI: 10.1093/jaoacint/qsad042
Menko van der Ark, Johan Hopman, Paul Mijland, Wubbo Mulder, Fatma Asdarci, Xavier O' Connell, Jelena Medic, Qian Wei, Kommer Brunt

Background: Propylene chlorohydrins (PCHs) are formed as byproducts in the reaction between starch and propylene oxide (PO). For hydroxypropylated (HP) starch applications in food, Joint FAO/WHO Expert Committee on Food additives (JECFA) set the maximum allowed total propylene chlorohydrin (PHC-t) residues level at 1 mg/kg.

Objective: To develop an improved analytical method for the determination of the PCH-t content in starches in the low mg/kg range to replace the outdated JECFA method.

Methods: A new GC-MS method that utilizes aqueous methanol as extraction medium for PCH. The GC-MS system is equipped with a programmable temperature vaporization injector and Stabilwax-DA column and uses helium as carrier gas. Quantitative detection is achieved in selected ion monitoring mode.

Results: This single-laboratory validation (SLV) study showed good linear calibrations for both 1-chloro-2-propanol (PCH-1) and 2-chloro-1-propanol (PCH-2) in the concentration range of 0.5-4 mg/kg in dry starch. The lower LOQ of PCH-1 and PCH-2 was 0.2-0.3 mg/kg in dry starch, the reproducibility RSD (RSDR) at the concentration level of 1-2 mg/kg in dry starch was 3-5%, and the recovery values for both PCH-1 and PCH-2 were in the range of 78-112% at a concentration level of about 0.6 mg/kg in dry starch. Compared with the current, outdated JECFA method, the new GC-MS method is more sustainable, less laborious, and therefore more economical. The analytical capacity of the new method is 4-5 times higher than the analytical capacity of the old JECFA method.

Conclusion: The GC-MS method is fit for a multi-laboratory trial (MLT).

Highlights: Based on the results of this SLV and the MLT (will be published in a second paper), the Joint FAO/WHO Expert Committee on Food Additives has recently decided to replace the outdated GC-FID JECFA method with the new GC-MS method for the determination of PCH-t content in starches.

背景:丙二氯丙烷(PCHs)是淀粉和环氧丙烷(PO)反应的副产物。对于在食品中应用的羟丙基化(HP)淀粉,粮农组织/世卫组织食品添加剂联合专家委员会(JECFA)将丙烯-氯丙烷(PHC-t)的最大允许残留量定为每公斤1毫克。目的:建立一种改进的低mg/kg范围内测定淀粉中PCH-t含量的分析方法,以取代过时的JECFA法。方法:采用气相色谱-质谱联用技术,以甲醇水溶液为提取介质提取PCH。GC-MS系统配备可编程温度汽化注射器和Stabilwax-DA柱,并使用氦气作为载气。定量检测在选定的离子监测模式下实现。结果:在0.5 ~ 4mg /kg的浓度范围内,对干淀粉中1-氯-2-丙醇(PCH-1)和2-氯-1-丙醇(PCH-2)均具有良好的线性校准效果。PCH-1和PCH-2在干淀粉中的下限限为0.2 ~ 0.3 mg/kg, 1 ~ 2 mg/kg干淀粉浓度下的重复性RSD (RSDR)为3 ~ 5%,在约0.6 mg/kg干淀粉浓度下,PCH-1和PCH-2的回收率在78 ~ 112%之间。与目前过时的JECFA方法相比,新的GC-MS方法更具可持续性,更省力,因此更经济。新方法的分析能力是旧方法的4-5倍。结论:气相色谱-质谱法适用于多实验室试验。根据SLV和MLT的结果(将在第二篇论文中发表),粮农组织/世卫组织食品添加剂联合专家委员会最近决定用新的GC-MS方法取代过时的GC-FID JECFA方法来测定淀粉中PCH-t的含量。
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引用次数: 0
Analytical Quality by Design-Driven RP-HPLC Method Conditions to Concomitantly Determine Cinnarizine and Morin Hydrate in Combined Drug Solution and Dual Drug-Loaded Formulations. 设计驱动反相高效液相色谱法测定复方和双载制剂中肉桂利嗪和水合莫宁的条件。
IF 1.6 4区 农林科学 Q2 Medicine Pub Date : 2023-09-01 DOI: 10.1093/jaoacint/qsad068
Abhinab Goswami, Syed Nazrin R Rahman, Datta M Pawde, Tamilvanan Shunmugaperumal

Background: The replacement of traditional oils with a camphor and menthol-based eutectic mixture is done to prepare oil-less emulsion-like dispersions for co-delivery of cinnarizine (CNZ) and morin hydrate (MH) for managing Meniére's disease (MD). Since two drugs are loaded into the dispersions, the development of a suitable reverse phase-high performance liquid chromatography (RP-HPLC) method for their simultaneous analysis becomes inevitable.

Objective: By applying the analytical quality by design (AQbD) approach, the RP-HPLC method conditions were optimized for the concomitant determination of two drugs.

Methods: The systematic AQbD started with identifying critical method attributes (CMA) through an Ishikawa fishbone diagram, risk estimation matrix, and risk priority number-based failure mode effect analysis followed by screening using fractional factorial design and optimization by face-centered central composite design. The concomitant determination of two drugs by the optimized RP-HPLC method condition was substantiated via specificity checking using combined drug solution, drug entrapment efficiency, and in vitro release of the two drugs from emulsion-like dispersions.

Results: The AQbD optimized RP-HPLC method conditions revealed the retention time for CNZ and MH at 5.017 and 5.323, respectively. The studied validation parameters were found within the ICH-prescribed limits. Exposing the individual drug solutions to acidic and basic hydrolytic conditions yielded extra chromatographic peaks for MH, probably due to the degradation of MH. The DEE % values of 87.40 ± 4.70 and 74.79 ± 2.94, respectively, were noticed for CNZ and MH in emulsion-like dispersions. More than 98% CNZ and MH release was occurred from emulsion-like dispersions within 30 min post-dissolution in artificial perilymph.

Conclusions: Overall, the AQbD approach could be helpful for systematic optimization of RP-HPLC method conditions to estimate concomitantly other therapeutic moieties.

Highlights: The proposed article shows the successful application of AQbD for the optimization of RP-HPLC method conditions to concomitantly estimate CNZ and MH in combined drug solution and dual-drug-loaded emulsion-like dispersions.

背景:以樟脑和薄荷醇为基础的共晶混合物取代传统油,制备无油乳剂状分散体,用于联合递送肉桂嗪(CNZ)和水合桑胺(MH),以治疗menisamure病(MD)。由于两种药物被装载到分散体中,因此开发一种合适的反相高效液相色谱(RP-HPLC)方法来同时分析它们就成为必然。目的:采用设计质量法(AQbD),优化两种药物同时测定的反相高效液相色谱法条件。方法:系统AQbD首先通过石川鱼骨图、风险估计矩阵和基于风险优先级数的失效模式效应分析识别关键方法属性(CMA),然后采用分数析因设计进行筛选,再采用面心中心复合设计进行优化。通过联合药液的特异性检查、药物包封效率检查和两种药物在乳状分散体中的体外释放度检查,验证了优化后的反相高效液相色谱法条件下两种药物的同时测定。结果:AQbD优化的反相高效液相色谱法条件下,CNZ和MH的保留时间分别为5.017和5.323。所研究的验证参数均在ich规定的限度内。将单个药物溶液暴露于酸性和碱性水解条件下,可能是由于MH的降解,产生了额外的MH色谱峰。在乳状分散体中,CNZ和MH的DEE %分别为87.40±4.70和74.79±2.94。乳状分散体在人工淋巴周围溶出后30 min内释放出98%以上的CNZ和MH。结论:总体而言,AQbD方法有助于系统优化RP-HPLC方法条件,以估计伴随的其他治疗成分。重点:本文成功应用AQbD优化RP-HPLC法同时测定复方药物溶液和双载乳状分散体中CNZ和MH的条件。
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引用次数: 0
An Antiviral Drug-Peramivir: Degradation and Identification of Impurities and the Endorsement of an HPLC-MS Method. 抗病毒药物帕拉米韦:杂质的降解和鉴定及高效液相色谱-质谱法的认可。
IF 1.6 4区 农林科学 Q2 Medicine Pub Date : 2023-09-01 DOI: 10.1093/jaoacint/qsad046
Thulaseedhar Alumuri, Karuna Sree Merugu, L A Amarababu Namburi, Aravınd Kurnool, Arunachalam SaravanaVadivu, Selvakumar Balasubramanian

Background: Peramivir is a neuraminidase inhibitor that serves as a transition state analogue for influenza neuraminidase, inhibiting the formation of new viruses in infected cells, and has been approved for intravenous administration.

Objective: To validate an HPLC method used to identify the degraded products of the antiviral drug peramivir.

Methods: Herein, we report the identification of compounds formed after the degradation of peramivir through acid, alkali, peroxide, thermal, and photolytic degradation. At the level of toxicology, a technique was devised for the isolation and measurement of peramivir.

Results: A sensitive and reliable LC-tandem mass spectrometry technique for the quantitative measurement of Peramivir and its impurities was developed and verified in order to comply with the recommendations made by the International Council for Harmonisation (ICH). The proposed protocol was in the 50-750 µg/mL range. Relative Standard Deviation values of less than 2.0% indicated good recovery in the range of 98.36-102.57%. Within the studied range, the calibration curves demonstrated good linearity and, in addition, the fitting of correlation coefficient was more than 0.999 for every impurity. Quantitative analysis of contaminants revealed the high efficiency at a low level.

Conclusion: Given its ability to separate degradation products, quantitative analysis is used to detect and quantify known and unknown impurities and degradants in the peramivir drug substance during routine analysis and stability studies. No significant degradation was found in peroxide and photolytic degradation studies.

Highlights: An HPLC method was developed and put to the test in order to analyze the behavior of the impurities of peramivir as they degraded when subjected to the stress conditions suggested by the ICH. Peramivir was found to be stable under peroxide and photolysis conditions but not stable or degradable when exposed to the acid, base, and thermal stress conditions. The method developed was extremely precise, linear, accurate, robust, and rugged. As a result, this technology has the potential to be used in the medication production process for regular impurity analysis as well as for the stability analysis of peramivir.

背景:Peramivir是一种神经氨酸酶抑制剂,作为流感神经氨酸酶的过渡状态类似物,抑制感染细胞中新病毒的形成,已被批准用于静脉注射。目的:建立高效液相色谱法鉴别抗病毒药物帕拉米韦降解产物的方法。方法:本文报道了帕拉米韦经酸、碱、过氧化物、热和光解降解后形成的化合物的鉴定。在毒理学水平上,设计了一种分离和测定帕拉米韦的技术。结果:建立了一种灵敏可靠的液相色谱-串联质谱法定量测定帕拉米韦及其杂质的方法,并经验证符合国际协调理事会(ICH)的建议。提议的方案在50-750µg/mL范围内。相对标准偏差小于2.0%,回收率为98.36 ~ 102.57%。在研究范围内,各杂质的线性关系良好,相关系数均在0.999以上。污染物的定量分析表明,该方法在低水平下效率高。结论:鉴于其降解产物的分离能力,在常规分析和稳定性研究中,定量分析可用于检测和定量帕拉米韦原料药中已知和未知的杂质和降解物。在过氧化和光解降解研究中没有发现明显的降解。重点:建立了高效液相色谱法,并进行了测试,以分析帕拉米韦中杂质在ICH建议的应激条件下降解的行为。Peramivir在过氧化和光解条件下是稳定的,但在酸、碱和热应力条件下不稳定或可降解。所开发的方法非常精确,线性,准确,坚固耐用。因此,该技术有潜力用于药物生产过程中的常规杂质分析以及帕拉米韦的稳定性分析。
{"title":"An Antiviral Drug-Peramivir: Degradation and Identification of Impurities and the Endorsement of an HPLC-MS Method.","authors":"Thulaseedhar Alumuri,&nbsp;Karuna Sree Merugu,&nbsp;L A Amarababu Namburi,&nbsp;Aravınd Kurnool,&nbsp;Arunachalam SaravanaVadivu,&nbsp;Selvakumar Balasubramanian","doi":"10.1093/jaoacint/qsad046","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad046","url":null,"abstract":"<p><strong>Background: </strong>Peramivir is a neuraminidase inhibitor that serves as a transition state analogue for influenza neuraminidase, inhibiting the formation of new viruses in infected cells, and has been approved for intravenous administration.</p><p><strong>Objective: </strong>To validate an HPLC method used to identify the degraded products of the antiviral drug peramivir.</p><p><strong>Methods: </strong>Herein, we report the identification of compounds formed after the degradation of peramivir through acid, alkali, peroxide, thermal, and photolytic degradation. At the level of toxicology, a technique was devised for the isolation and measurement of peramivir.</p><p><strong>Results: </strong>A sensitive and reliable LC-tandem mass spectrometry technique for the quantitative measurement of Peramivir and its impurities was developed and verified in order to comply with the recommendations made by the International Council for Harmonisation (ICH). The proposed protocol was in the 50-750 µg/mL range. Relative Standard Deviation values of less than 2.0% indicated good recovery in the range of 98.36-102.57%. Within the studied range, the calibration curves demonstrated good linearity and, in addition, the fitting of correlation coefficient was more than 0.999 for every impurity. Quantitative analysis of contaminants revealed the high efficiency at a low level.</p><p><strong>Conclusion: </strong>Given its ability to separate degradation products, quantitative analysis is used to detect and quantify known and unknown impurities and degradants in the peramivir drug substance during routine analysis and stability studies. No significant degradation was found in peroxide and photolytic degradation studies.</p><p><strong>Highlights: </strong>An HPLC method was developed and put to the test in order to analyze the behavior of the impurities of peramivir as they degraded when subjected to the stress conditions suggested by the ICH. Peramivir was found to be stable under peroxide and photolysis conditions but not stable or degradable when exposed to the acid, base, and thermal stress conditions. The method developed was extremely precise, linear, accurate, robust, and rugged. As a result, this technology has the potential to be used in the medication production process for regular impurity analysis as well as for the stability analysis of peramivir.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10514703","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 CompactDry "Nissui" BC for Enumeration of Bacillus cereus in a Variety of Foods: AOAC Performance Tested MethodSM 092201. 用于多种食品中蜡样芽孢杆菌计数的CompactDry“Nissui”BC的验证:AOAC性能测试方法sm 092201。
IF 1.6 4区 农林科学 Q2 Medicine Pub Date : 2023-09-01 DOI: 10.1093/jaoacint/qsad045
Yusuke Koyanagi, Tomoki Yamazaki, Gail Betts

Background: The CompactDry "Nissui" BC is a ready-to-use dry media sheet using a chromogenic medium with selective agents for the detection and enumeration of Bacillus cereus in products after incubation at 30 ± 1°C for 24 ± 2 h.

Objective: The CompactDry "Nissui" BC method was validated to achieve AOAC Performance Tested MethodsSM certification.

Method: The performance of the CompactDry "Nissui" BC was compared to that of ISO 7932:2004 for 10 matrixes, including panna cotta, double cream, dried baby food, dried vegetable soup mix, seafood sticks, salmon pâté, sliced ham, pork liver pâté, ham and cheese sandwich, and Caesar pasta salad with chicken and bacon. Performance indicators included repeatability, difference of means (DOM), and inclusivity/exclusivity.

Results: After log10 transformation of the data, the relative standard deviation of repeatability (RSDr) was ≤9.2% for 28 of the 30 materials (10 matrixes each at three contamination levels) analyzed by the CompactDry "Nissui" BC method and ≤13% for 27 of the 30 matrix/level combinations analyzed by the reference method. Method equivalence was demonstrated in 28 of the 30 matrix/level combinations based on the 90% confidence interval of the DOM being within (-0.5, 0.5). For inclusivity, 47 of 50 strains tested showed typical colonies and confirmed positive. For exclusivity, 28 of 33 strains tested resulted in no growth or were negative, and five were positive. Inclusivity and exclusivity results were similar on the reference method agar. The method was shown to be robust to changes in sample volume, incubation temperature, and incubation time, and data are presented supporting product consistency and 18-month shelf life.

Conclusions: The CompactDry "Nissui" BC method is validated for the determination of Bacillus cereus in a variety of matrixes.

Highlights: The CompactDry "Nissui" BC method is equivalent to the ISO 7932:2004 reference method and is suitable for Performance Tested MethodsSM certification for the matrixes tested.

背景:CompactDry“Nissui”BC是一种即用型干培养基,使用带有选择性试剂的显色培养基,在30±1℃孵育24±2小时后,用于检测和枚举蜡样芽孢杆菌。目的:验证CompactDry“Nissui”BC法获得AOAC性能测试方法ssm认证。方法:将CompactDry“Nissui”BC与ISO 7932:2004对panna cotta、双层奶油、婴儿食品干、蔬菜干汤、海鲜棒、三文鱼粉、火腿片、猪肝粉、火腿芝士三明治、鸡肉培根凯撒意面沙拉等10种基质的性能进行比较。性能指标包括可重复性、均数差异(DOM)和包容性/排他性。结果:对数据进行log10变换后,CompactDry“Nissui”BC法分析的30种材料(3种污染水平各10种基质)中有28种重复性相对标准偏差(RSDr)≤9.2%,参考法分析的30种基质/水平组合中有27种重复性相对标准偏差≤13%。基于DOM的90%置信区间在(-0.5,0.5)内,30个矩阵/层组合中的28个证明了方法等价性。在包容性方面,测试的50株菌株中有47株显示典型菌落并确诊为阳性。在排他性方面,33个菌株中有28个没有生长或呈阴性,5个呈阳性。在对照法琼脂上的包容性和排他性结果相似。该方法对样品体积、孵育温度和孵育时间的变化具有鲁棒性,并提供了支持产品一致性和18个月保质期的数据。结论:CompactDry“Nissui”BC法可用于多种基质中蜡样芽孢杆菌的检测。重点:CompactDry“Nissui”BC方法相当于ISO 7932:2004参考方法,适用于测试矩阵的性能测试方法ssm认证。
{"title":"Validation of the CompactDry \"Nissui\" BC for Enumeration of Bacillus cereus in a Variety of Foods: AOAC Performance Tested MethodSM 092201.","authors":"Yusuke Koyanagi,&nbsp;Tomoki Yamazaki,&nbsp;Gail Betts","doi":"10.1093/jaoacint/qsad045","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad045","url":null,"abstract":"<p><strong>Background: </strong>The CompactDry \"Nissui\" BC is a ready-to-use dry media sheet using a chromogenic medium with selective agents for the detection and enumeration of Bacillus cereus in products after incubation at 30 ± 1°C for 24 ± 2 h.</p><p><strong>Objective: </strong>The CompactDry \"Nissui\" BC method was validated to achieve AOAC Performance Tested MethodsSM certification.</p><p><strong>Method: </strong>The performance of the CompactDry \"Nissui\" BC was compared to that of ISO 7932:2004 for 10 matrixes, including panna cotta, double cream, dried baby food, dried vegetable soup mix, seafood sticks, salmon pâté, sliced ham, pork liver pâté, ham and cheese sandwich, and Caesar pasta salad with chicken and bacon. Performance indicators included repeatability, difference of means (DOM), and inclusivity/exclusivity.</p><p><strong>Results: </strong>After log10 transformation of the data, the relative standard deviation of repeatability (RSDr) was ≤9.2% for 28 of the 30 materials (10 matrixes each at three contamination levels) analyzed by the CompactDry \"Nissui\" BC method and ≤13% for 27 of the 30 matrix/level combinations analyzed by the reference method. Method equivalence was demonstrated in 28 of the 30 matrix/level combinations based on the 90% confidence interval of the DOM being within (-0.5, 0.5). For inclusivity, 47 of 50 strains tested showed typical colonies and confirmed positive. For exclusivity, 28 of 33 strains tested resulted in no growth or were negative, and five were positive. Inclusivity and exclusivity results were similar on the reference method agar. The method was shown to be robust to changes in sample volume, incubation temperature, and incubation time, and data are presented supporting product consistency and 18-month shelf life.</p><p><strong>Conclusions: </strong>The CompactDry \"Nissui\" BC method is validated for the determination of Bacillus cereus in a variety of matrixes.</p><p><strong>Highlights: </strong>The CompactDry \"Nissui\" BC method is equivalent to the ISO 7932:2004 reference method and is suitable for Performance Tested MethodsSM certification for the matrixes tested.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10142542","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 a Rapid Microbiological Method for the Detection and Quantification of the Burkholderia cepacia Complex in an Antacid Oral Suspension. 抗酸口服混悬液中洋葱伯克氏菌复合体快速检测和定量的微生物学方法验证。
IF 1.6 4区 农林科学 Q2 Medicine Pub Date : 2023-09-01 DOI: 10.1093/jaoacint/qsad056
Harold A Prada-Ramírez, Sandra Celeita, Juan Camilo Fonseca

Background: Despite the broad adoption of Soleris® technology in the food industry as semiquantitative method, it is almost completely unexplored in the pharmaceutical industry as a quantitative method for quantification of Burkholderia cepacia complex (Bcc).

Objective: The efficacy of an automated growth-based system for a quantitative determination of the Bcc in an antacid oral suspension was studied. The main purpose of this validation study was to prove that the alternative method's entire performance is not inferior to the conventional method for a quantitative determination of Bcc.

Method: The antacid oral suspension's preservatives were neutralized, leading to the Burkholderia complex's recovery by means of the alternative method and the reference method. A calibration curve was generated for each strain by plotting DTs relative to the corresponding log CFU values. An equivalence of results was done through the construction of calibration curves that allowed the establishment of numerically equivalent results between the enumeration data from the reference method and the alternative method.

Results: Thus following the guidelines of USP, essential validation parameters were shown, such as equivalence of results (CC >0.95), linearity (R2 >0.9025), accuracy (% recovery >70%), operating range, precision and ruggedness (DS <5 and CV <35%), specificity (inclusivity and exclusivity), limit of detection (LOD), and limit of quantification (LOQ).

Conclusions: It was shown that all the test results obtained from the alternative method were in statistical agreement with the standard method. Thus this new technology was found to meet all the validation criteria needed to be considered as an alternative method for the quantification of the Burkholderia complex in the antacid oral suspension tested.

Highlights: As outlined in USP chapter <1223> and demonstrated in this research the implementation of alternative methods can offer benefits in execution and automation while improving accuracy, sensitivity, and precision and can reduce the microbiological process time compared to the traditional ones.

背景:尽管Soleris技术作为半定量方法在食品工业中被广泛采用,但在制药工业中,作为洋葱伯克霍尔德菌复合体(Bcc)的定量方法,它几乎完全没有被探索过。目的:研究基于生长的自动系统定量测定抗酸口服混悬液中Bcc的效果。本验证研究的主要目的是证明替代方法的整体性能不低于常规方法用于Bcc的定量测定。方法:采用替代法和参比法对抗酸口服混悬液中的防腐剂进行中和,使伯克霍尔德菌复体恢复。通过绘制dt相对于相应的对数CFU值生成每个应变的校准曲线。通过建立校准曲线,使参考方法和备选方法的枚举数据在数值上等效。结果:在USP的指导下,给出了基本的验证参数,如结果的等效性(CC >0.95)、线性度(R2 >0.9025)、准确度(回收率>70%)、工作范围、精密度和坚固性(DS)。结论:替代方法得到的所有试验结果与标准方法在统计学上一致。因此,这项新技术被发现满足所有的验证标准,需要考虑作为一种替代方法,定量伯克霍尔德菌复合体在抗酸口服混悬液测试。要点:正如USP章节所概述的和本研究中所展示的,替代方法的实施可以在执行和自动化方面提供好处,同时提高准确性,灵敏度和精度,并且与传统方法相比可以减少微生物处理时间。
{"title":"Validation of a Rapid Microbiological Method for the Detection and Quantification of the Burkholderia cepacia Complex in an Antacid Oral Suspension.","authors":"Harold A Prada-Ramírez,&nbsp;Sandra Celeita,&nbsp;Juan Camilo Fonseca","doi":"10.1093/jaoacint/qsad056","DOIUrl":"https://doi.org/10.1093/jaoacint/qsad056","url":null,"abstract":"<p><strong>Background: </strong>Despite the broad adoption of Soleris® technology in the food industry as semiquantitative method, it is almost completely unexplored in the pharmaceutical industry as a quantitative method for quantification of Burkholderia cepacia complex (Bcc).</p><p><strong>Objective: </strong>The efficacy of an automated growth-based system for a quantitative determination of the Bcc in an antacid oral suspension was studied. The main purpose of this validation study was to prove that the alternative method's entire performance is not inferior to the conventional method for a quantitative determination of Bcc.</p><p><strong>Method: </strong>The antacid oral suspension's preservatives were neutralized, leading to the Burkholderia complex's recovery by means of the alternative method and the reference method. A calibration curve was generated for each strain by plotting DTs relative to the corresponding log CFU values. An equivalence of results was done through the construction of calibration curves that allowed the establishment of numerically equivalent results between the enumeration data from the reference method and the alternative method.</p><p><strong>Results: </strong>Thus following the guidelines of USP, essential validation parameters were shown, such as equivalence of results (CC >0.95), linearity (R2 >0.9025), accuracy (% recovery >70%), operating range, precision and ruggedness (DS <5 and CV <35%), specificity (inclusivity and exclusivity), limit of detection (LOD), and limit of quantification (LOQ).</p><p><strong>Conclusions: </strong>It was shown that all the test results obtained from the alternative method were in statistical agreement with the standard method. Thus this new technology was found to meet all the validation criteria needed to be considered as an alternative method for the quantification of the Burkholderia complex in the antacid oral suspension tested.</p><p><strong>Highlights: </strong>As outlined in USP chapter <1223> and demonstrated in this research the implementation of alternative methods can offer benefits in execution and automation while improving accuracy, sensitivity, and precision and can reduce the microbiological process time compared to the traditional ones.</p>","PeriodicalId":15003,"journal":{"name":"Journal of AOAC International","volume":null,"pages":null},"PeriodicalIF":1.6,"publicationDate":"2023-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10132978","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: 1
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