Pub Date : 2024-09-18DOI: 10.2174/0115734129317487240906073916
Zhang Qiao, Shen Mengmeng, Zhu Li, Xiao Chaoqiang, He Shuwang, Yang Jie
Background: Vitamin A and D deficiency in children is a common public health problem. In China, almost all children are administered vitamin A and D preparations daily and over the long term. Children are sensitive to elemental impurities, including heavy metals. However, there are no regulatory requirements or reports on the risk assessment of elemental impurities in marketed vitamin A and D preparations. Objective: The aim of this study was to propose an accurate and efficient method suitable for samples from different manufacturers to detect elemental impurities and conduct risk assessments according to the ICH Q3D guidelines. Methods: We developed a universally applicable digestion method for capsules and an ICP–MS method for quantitative analysis of 28 elemental impurities in vitamin A and D formulations. These methods were validated according to the USP 233 guidelines. Elemental impurities in 15 batches of vitamin A and D products from 10 manufacturers and their capsule shells were determined, and risk assessment was conducted according to the International Council for Harmonization Q3D guidelines. Results: All elemental impurities of toxicological concern met the Q3D requirements. However, the concentrations of various elements, including those of lead (not detected to 4.1 µg/g), arsenic (not detected to 7 µg/g), aluminum (not detected to 888 µg/g), and palladium (not detected to 36 µg/g), varied markedly. Moreover, the lead content in one batch from one manufacturer exceeded the control threshold. Conclusion: In this study, we successfully developed an effective digestion method for processing capsules containing samples from different sources and a sensitive ICP–MS method for quantitative determination of 28 elemental impurities in vitamin A and D preparations. ICP–MS should be implemented for the evaluation and control of elemental impurities in vitamin A and D preparations. This will ensure safe long-term vitamin A and D supplementation in children
背景：儿童维生素 A 和 D 缺乏是一个常见的公共卫生问题。在中国，几乎所有儿童每天都要长期服用维生素 A 和 D 制剂。儿童对重金属等元素杂质非常敏感。然而，目前还没有关于市售维生素 A 和 D 制剂中元素杂质风险评估的法规要求或报告。研究目的本研究旨在根据 ICH Q3D 指南，提出一种适用于不同生产商样品的准确、高效的元素杂质检测方法，并进行风险评估。方法：我们开发了一种普遍适用的胶囊消化方法和一种 ICP-MS 方法，用于定量分析维生素 A 和 D 配方中的 28 种元素杂质。这些方法根据 USP 233 准则进行了验证。测定了 10 家制造商生产的 15 批维生素 A 和 D 产品及其胶囊壳中的元素杂质，并根据国际协调理事会 Q3D 准则进行了风险评估。结果显示所有引起毒理学关注的元素杂质均符合 Q3D 要求。不过，各种元素的浓度差异明显，包括铅（未检出至 4.1 微克/克）、砷（未检出至 7 微克/克）、铝（未检出至 888 微克/克）和钯（未检出至 36 微克/克）。此外，一家制造商生产的一批产品中的铅含量超过了控制阈值。结论在这项研究中，我们成功地开发了一种有效的消化方法来处理含有不同来源样品的胶囊，并开发了一种灵敏的 ICP-MS 方法来定量测定维生素 A 和维生素 D 制剂中的 28 种元素杂质。ICP-MS 应用于维生素 A 和 D 制剂中元素杂质的评估和控制。这将确保儿童长期安全地补充维生素 A 和 D。
{"title":"Universally Applicable Methods for Comprehensive Risk Assessment of Elemental Impurities in Vitamin A and D Preparations","authors":"Zhang Qiao, Shen Mengmeng, Zhu Li, Xiao Chaoqiang, He Shuwang, Yang Jie","doi":"10.2174/0115734129317487240906073916","DOIUrl":"https://doi.org/10.2174/0115734129317487240906073916","url":null,"abstract":"Background: Vitamin A and D deficiency in children is a common public health problem. In China, almost all children are administered vitamin A and D preparations daily and over the long term. Children are sensitive to elemental impurities, including heavy metals. However, there are no regulatory requirements or reports on the risk assessment of elemental impurities in marketed vitamin A and D preparations. Objective: The aim of this study was to propose an accurate and efficient method suitable for samples from different manufacturers to detect elemental impurities and conduct risk assessments according to the ICH Q3D guidelines. Methods: We developed a universally applicable digestion method for capsules and an ICP–MS method for quantitative analysis of 28 elemental impurities in vitamin A and D formulations. These methods were validated according to the USP 233 guidelines. Elemental impurities in 15 batches of vitamin A and D products from 10 manufacturers and their capsule shells were determined, and risk assessment was conducted according to the International Council for Harmonization Q3D guidelines. Results: All elemental impurities of toxicological concern met the Q3D requirements. However, the concentrations of various elements, including those of lead (not detected to 4.1 µg/g), arsenic (not detected to 7 µg/g), aluminum (not detected to 888 µg/g), and palladium (not detected to 36 µg/g), varied markedly. Moreover, the lead content in one batch from one manufacturer exceeded the control threshold. Conclusion: In this study, we successfully developed an effective digestion method for processing capsules containing samples from different sources and a sensitive ICP–MS method for quantitative determination of 28 elemental impurities in vitamin A and D preparations. ICP–MS should be implemented for the evaluation and control of elemental impurities in vitamin A and D preparations. This will ensure safe long-term vitamin A and D supplementation in children","PeriodicalId":10889,"journal":{"name":"Current Pharmaceutical Analysis","volume":"37 1","pages":""},"PeriodicalIF":0.6,"publicationDate":"2024-09-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142264823","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-18DOI: 10.2174/0115734129286160240909063156
Chao Chen, Yan Wang, Yue Chen, Aijing Zhang, Zhiwei Cai, Lei Cheng, Bingyong Xu, Xinyou Bao, Jianmou Liang
aims: To establish a GC-MS method for the determination of extractable substances in the stoppers of Ceftriaxone sodium bottles for injection; To establish a HPLC method for the determination of vulcanizing agent and antioxidant in Ceftriaxone sodium for injection bottle stopper and to analyze the correlation between the volatile substances of rubber stopper and the clarity of solution. objective: To establish a GC-MS method for the determination of extractable substances in the stoppers of Ceftriaxone sodium bottles for injection; To establish a HPLC method for the determination of vulcanizing agent and antioxidant in Ceftriaxone sodium for injection bottle stopper and to analyze the correlation between the volatile substances of rubber stopper and the clarity of solution. method: GC-MS method was used with capillary column Rtx-5MS (30.0 m×0.25 mm, 0.25 µm), the carrier gas was He at the flow rate of 1.8mL·min-1, the temperature of injection port was 200 ℃, shunt ratio was 10∶l, the column temperature was programmed temperature(initial column temperature was 40 ℃ and kept for 15 min, and with the speed of 10 ℃ upping to 100 ℃ and kept for 2 min, and with the speed of 25 ℃ upping to 230 ℃ and kept for 10 min), the interface temperature was 250 ℃, and the scanning range was from 29 to 600(m·z-1), and the volatile substances were using full scan. An inertsil ODS-3 column(250 mm×4.6 mm, 5 µm) was used for the HPLC analysis. The mobile phase A consisted of water containing 0.04% trifluoroacetic and the mobile phase B consisted of acetonitrile containing 0.04% trifluoroacetic acid, the gradient elution was used and the flow rate was set as 1.0 mL·min-1. The column temperature was 30 ℃, the detection wavelength was 210 nm and the injection volume was 10 µL. result: Antioxidant BHT(264), silicone oil and other organic compounds in rubber stopper permeated and migrated to the sample with acceleration time by GC-MS. A good linearity was observed over the range of 0.5-100 μg·mL-1(r＞0.999). The detection limits of vulcanizing agent and antioxidant were about 0.03 μg·mL-1, and the quantitation limits were about 0.1 μg·mL-1. The average recoveries (low, medium and high) of antioxidant (168, 264, 330, 1076, 1010) and vulcanizing agents (carbon disulfide, sulfur) were between 90.0% and 110.0%, and the corresponding RSD were less than 5% (n=9) by adding standard recovery experiments. The stability test showed that the antioxidant and the vulcanizing agent solution had good stability and was stable within 24 hours. conclusion: the GC-MS/HPLC method can be used for the quality control of rubber stopper of cefuroxime Sodium for Injection.The compatibility study and comprehensive evaluation system of Ceftriaxone sodium for injection packaging materials have been initially formed.
{"title":"Research on Compatibility of Packaging Materials of High-Risk Cephalosporin Powder Injection and Establishment of Indicator Component Evaluation Method","authors":"Chao Chen, Yan Wang, Yue Chen, Aijing Zhang, Zhiwei Cai, Lei Cheng, Bingyong Xu, Xinyou Bao, Jianmou Liang","doi":"10.2174/0115734129286160240909063156","DOIUrl":"https://doi.org/10.2174/0115734129286160240909063156","url":null,"abstract":"aims: To establish a GC-MS method for the determination of extractable substances in the stoppers of Ceftriaxone sodium bottles for injection; To establish a HPLC method for the determination of vulcanizing agent and antioxidant in Ceftriaxone sodium for injection bottle stopper and to analyze the correlation between the volatile substances of rubber stopper and the clarity of solution. objective: To establish a GC-MS method for the determination of extractable substances in the stoppers of Ceftriaxone sodium bottles for injection; To establish a HPLC method for the determination of vulcanizing agent and antioxidant in Ceftriaxone sodium for injection bottle stopper and to analyze the correlation between the volatile substances of rubber stopper and the clarity of solution. method: GC-MS method was used with capillary column Rtx-5MS (30.0 m×0.25 mm, 0.25 µm), the carrier gas was He at the flow rate of 1.8mL·min-1, the temperature of injection port was 200 ℃, shunt ratio was 10∶l, the column temperature was programmed temperature(initial column temperature was 40 ℃ and kept for 15 min, and with the speed of 10 ℃ upping to 100 ℃ and kept for 2 min, and with the speed of 25 ℃ upping to 230 ℃ and kept for 10 min), the interface temperature was 250 ℃, and the scanning range was from 29 to 600(m·z-1), and the volatile substances were using full scan. An inertsil ODS-3 column(250 mm×4.6 mm, 5 µm) was used for the HPLC analysis. The mobile phase A consisted of water containing 0.04% trifluoroacetic and the mobile phase B consisted of acetonitrile containing 0.04% trifluoroacetic acid, the gradient elution was used and the flow rate was set as 1.0 mL·min-1. The column temperature was 30 ℃, the detection wavelength was 210 nm and the injection volume was 10 µL. result: Antioxidant BHT(264), silicone oil and other organic compounds in rubber stopper permeated and migrated to the sample with acceleration time by GC-MS. A good linearity was observed over the range of 0.5-100 μg·mL-1(r＞0.999). The detection limits of vulcanizing agent and antioxidant were about 0.03 μg·mL-1, and the quantitation limits were about 0.1 μg·mL-1. The average recoveries (low, medium and high) of antioxidant (168, 264, 330, 1076, 1010) and vulcanizing agents (carbon disulfide, sulfur) were between 90.0% and 110.0%, and the corresponding RSD were less than 5% (n=9) by adding standard recovery experiments. The stability test showed that the antioxidant and the vulcanizing agent solution had good stability and was stable within 24 hours. conclusion: the GC-MS/HPLC method can be used for the quality control of rubber stopper of cefuroxime Sodium for Injection.The compatibility study and comprehensive evaluation system of Ceftriaxone sodium for injection packaging materials have been initially formed.","PeriodicalId":10889,"journal":{"name":"Current Pharmaceutical Analysis","volume":"36 1","pages":""},"PeriodicalIF":0.6,"publicationDate":"2024-09-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142264822","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-18DOI: 10.2174/0115734129321062240906070516
Vaishnavi A. Gosavi, Mahesh M. Deshpande, Gauri D. Ghangale, Machindra J. Chavan
Objective: A novel stability indicating RP-HPLC method was developed and validated for the simultaneous estimation of Pregabalin and Duloxetine by using the QBD approach. Method: To determine the optimal parameters for the duloxetine and pregabalin study, we used Design Expert version 13.0 in this work. The mobile phase consisted of 0.8 ml/min of methanol: water (80:20, v/v) with o-phosphoric acid-adjusted pH 3.A 250 mm × 4.6 mm ID, 5 μm particle size Cosmosil C18 column was used. The UV-3000-M detector was used to detect at 218 nm. Results: Duloxetine's retention time was 7.153 ±0.1 min, whereas Pregabalin's was 4.481±0.1 min. The ICH parameters like linearity, accuracy, robustness, ruggedness, LOD and LOQ, and system suitability were determined. Likewise, the tailing factors were found to be 1.27 and 1.26, while the theoretical plates of duloxetine and pregabalin were found to be 8313 and 8549, respectively. The recovery study shows the results (99.37–99.84% for pregabalin and 99.03–99.74% for duloxetine), and the precision was obtained with a %RSD of less than 2%. The result of the assay was 99.92 % for pregabalin and 99.39% for duloxetine. The developed method was used for the forced degradation study. The Box-Behnken design experiment using Design Expert 13.0 was adopted for the QBD approach. Conclusion: All the values obtained for different parameters were within the acceptable range of ICH. The developed method can be routinely used for the simultaneous estimation of Pregabalin and Duloxetine by using the QBD approach.
{"title":"Simultaneous Estimation of Pregabalin and Duloxetine Used to Treat Nerve Pain by Stability Indicating RP-HPLC Method Using the QBD Approach","authors":"Vaishnavi A. Gosavi, Mahesh M. Deshpande, Gauri D. Ghangale, Machindra J. Chavan","doi":"10.2174/0115734129321062240906070516","DOIUrl":"https://doi.org/10.2174/0115734129321062240906070516","url":null,"abstract":"Objective: A novel stability indicating RP-HPLC method was developed and validated for the simultaneous estimation of Pregabalin and Duloxetine by using the QBD approach. Method: To determine the optimal parameters for the duloxetine and pregabalin study, we used Design Expert version 13.0 in this work. The mobile phase consisted of 0.8 ml/min of methanol: water (80:20, v/v) with o-phosphoric acid-adjusted pH 3.A 250 mm × 4.6 mm ID, 5 μm particle size Cosmosil C18 column was used. The UV-3000-M detector was used to detect at 218 nm. Results: Duloxetine's retention time was 7.153 ±0.1 min, whereas Pregabalin's was 4.481±0.1 min. The ICH parameters like linearity, accuracy, robustness, ruggedness, LOD and LOQ, and system suitability were determined. Likewise, the tailing factors were found to be 1.27 and 1.26, while the theoretical plates of duloxetine and pregabalin were found to be 8313 and 8549, respectively. The recovery study shows the results (99.37–99.84% for pregabalin and 99.03–99.74% for duloxetine), and the precision was obtained with a %RSD of less than 2%. The result of the assay was 99.92 % for pregabalin and 99.39% for duloxetine. The developed method was used for the forced degradation study. The Box-Behnken design experiment using Design Expert 13.0 was adopted for the QBD approach. Conclusion: All the values obtained for different parameters were within the acceptable range of ICH. The developed method can be routinely used for the simultaneous estimation of Pregabalin and Duloxetine by using the QBD approach.","PeriodicalId":10889,"journal":{"name":"Current Pharmaceutical Analysis","volume":"189 1","pages":""},"PeriodicalIF":0.6,"publicationDate":"2024-09-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142264821","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-10DOI: 10.2174/0115734129317408240903150800
Filiz Demir, Raneen Albarri, Durişehvar Özer Ünal
: Biotechnology, a field discovered in 1919, unites biology and engineering to harness living organisms for medical purposes. Fueled by using DNA's discovery in the 1950s, biotechnology has converted through genetic engineering, yielding impactful merchandise regulated by means of entities like the FDA. The manufacturing involves upstream and downstream processing including the various techniques involved in the downstream processing of biotechnological drugs, along with relevant guidelines and chromatographic analysis methods. The biotechnological industry, which integrates biological science with engineering, has significantly advanced since the discovery of DNA's structure, leading to the development of biopharmaceuticals. These drugs, including monoclonal antibodies, recombinant proteins, and gene therapies, are produced using living organisms and hold the potential for treating complex diseases. The downstream process, a crucial phase in biopharmaceutical production, involves the purification and formulation of drug products to meet stringent regulatory standards. Traditional techniques such as centrifugation, filtration, and chromatography are employed to extract and purify biopharmaceuticals. Chromatographic techniques, including ion exchange, affinity, and size exclusion chromatography, play a pivotal role in achieving the desired purity levels. However, these methods are often time-- consuming and expensive, necessitating continuous advancements in the field. The paper highlights the importance of regulatory guidelines, including cGMP, in ensuring the quality and safety of biopharmaceuticals. It also discusses the significant role of organizations such as the FDA and EMA in regulating biotechnological drug production. The evolution of downstream processing techniques and the development of novel methods promise greater efficiency, scalability, and cost-effectiveness in biopharmaceutical production. Understanding these advancements is essential for continued growth and innovation in the industry, ultimately contributing to improved patient care and pharmaceutical innovation.
:生物技术是 1919 年发现的一个领域，它将生物学和工程学结合起来，将生物体用于医疗目的。在 20 世纪 50 年代 DNA 发现的推动下，生物技术通过基因工程进行了转换，产生了受美国食品及药物管理局等实体监管的有影响力的商品。生产涉及上游和下游加工，包括生物技术药物下游加工所涉及的各种技术，以及相关准则和色谱分析方法。生物技术产业是生物科学与工程学的结合，自发现 DNA 结构以来，生物技术产业取得了长足的进步，并由此开发出生物制药。这些药物包括单克隆抗体、重组蛋白和基因疗法，都是利用生物生产的，具有治疗复杂疾病的潜力。下游工艺是生物制药生产的关键阶段，包括药物产品的纯化和配制，以满足严格的监管标准。生物制药的提取和纯化采用离心、过滤和层析等传统技术。色谱技术，包括离子交换色谱、亲和色谱和尺寸排阻色谱，在达到所需的纯度水平方面发挥着关键作用。然而，这些方法往往耗时费钱，因此需要在这一领域不断取得进步。本文强调了包括 cGMP 在内的监管准则在确保生物制药质量和安全方面的重要性。论文还讨论了 FDA 和 EMA 等组织在监管生物技术药物生产方面的重要作用。下游加工技术的发展和新方法的开发有望提高生物制药生产的效率、可扩展性和成本效益。了解这些进步对行业的持续发展和创新至关重要，最终将有助于改善患者护理和医药创新。
{"title":"An Overview of Biotechnological Drug’s Various Techniques of Downstream Process, Guideline’s And Different Chromatographic Analysis","authors":"Filiz Demir, Raneen Albarri, Durişehvar Özer Ünal","doi":"10.2174/0115734129317408240903150800","DOIUrl":"https://doi.org/10.2174/0115734129317408240903150800","url":null,"abstract":": Biotechnology, a field discovered in 1919, unites biology and engineering to harness living organisms for medical purposes. Fueled by using DNA's discovery in the 1950s, biotechnology has converted through genetic engineering, yielding impactful merchandise regulated by means of entities like the FDA. The manufacturing involves upstream and downstream processing including the various techniques involved in the downstream processing of biotechnological drugs, along with relevant guidelines and chromatographic analysis methods. The biotechnological industry, which integrates biological science with engineering, has significantly advanced since the discovery of DNA's structure, leading to the development of biopharmaceuticals. These drugs, including monoclonal antibodies, recombinant proteins, and gene therapies, are produced using living organisms and hold the potential for treating complex diseases. The downstream process, a crucial phase in biopharmaceutical production, involves the purification and formulation of drug products to meet stringent regulatory standards. Traditional techniques such as centrifugation, filtration, and chromatography are employed to extract and purify biopharmaceuticals. Chromatographic techniques, including ion exchange, affinity, and size exclusion chromatography, play a pivotal role in achieving the desired purity levels. However, these methods are often time-- consuming and expensive, necessitating continuous advancements in the field. The paper highlights the importance of regulatory guidelines, including cGMP, in ensuring the quality and safety of biopharmaceuticals. It also discusses the significant role of organizations such as the FDA and EMA in regulating biotechnological drug production. The evolution of downstream processing techniques and the development of novel methods promise greater efficiency, scalability, and cost-effectiveness in biopharmaceutical production. Understanding these advancements is essential for continued growth and innovation in the industry, ultimately contributing to improved patient care and pharmaceutical innovation.","PeriodicalId":10889,"journal":{"name":"Current Pharmaceutical Analysis","volume":"10 1","pages":""},"PeriodicalIF":0.6,"publicationDate":"2024-09-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142181868","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-05DOI: 10.2174/0115734129319256240829053342
Anoop Kumar, Tanya Maheriya, Y. Madhu, K. Neetu, Harish Chander, Meena Kumari
Background: Purified human albumin fractionated from plasma has a complex matrix that imposes a lot of interference in quality control testing, particularly for impurities at trace level. In this study, a simple approach has been studied and validated for the quantification of aluminium content using Graphite Furnace Atomic Absorption Spectrometry (GF-AAS). As per international guidelines, the linearity, accuracy, precision, specificity, limit of detection, and quantification have been assessed. Results: The linearity of the analyte response was evaluated over the range of concentrations from 5μg/L to 45 μg/L, and the correlation coefficient obtained was greater than 0.99. The mean recovery obtained for the accuracy ranged from 102.29% to 106.81% at three concentration levels. The specificity/selectivity evaluated for possible interference from other metal ions and relative standard deviation for the high and low content was 10.24% and 6.50%, respectively, which was statistically verified and not significant. Method precision was evaluated for repeatability and intermediate precision, and the relative standard deviation obtained was 1.83% and 4.61%, respectively. The limit of detection and quantification obtained was 1.30 μg/L and 4.10 μg/L, respectively. Conclusion: Results obtained for the method performance show the suitability of the method for aluminium estimation in human albumin samples and should be used to control the limit of aluminium in human albumin blood products.
{"title":"Validation of GF-AAS Method for the Determination of Aluminium Content in Human Albumin Finished Product","authors":"Anoop Kumar, Tanya Maheriya, Y. Madhu, K. Neetu, Harish Chander, Meena Kumari","doi":"10.2174/0115734129319256240829053342","DOIUrl":"https://doi.org/10.2174/0115734129319256240829053342","url":null,"abstract":"Background: Purified human albumin fractionated from plasma has a complex matrix that imposes a lot of interference in quality control testing, particularly for impurities at trace level. In this study, a simple approach has been studied and validated for the quantification of aluminium content using Graphite Furnace Atomic Absorption Spectrometry (GF-AAS). As per international guidelines, the linearity, accuracy, precision, specificity, limit of detection, and quantification have been assessed. Results: The linearity of the analyte response was evaluated over the range of concentrations from 5μg/L to 45 μg/L, and the correlation coefficient obtained was greater than 0.99. The mean recovery obtained for the accuracy ranged from 102.29% to 106.81% at three concentration levels. The specificity/selectivity evaluated for possible interference from other metal ions and relative standard deviation for the high and low content was 10.24% and 6.50%, respectively, which was statistically verified and not significant. Method precision was evaluated for repeatability and intermediate precision, and the relative standard deviation obtained was 1.83% and 4.61%, respectively. The limit of detection and quantification obtained was 1.30 μg/L and 4.10 μg/L, respectively. Conclusion: Results obtained for the method performance show the suitability of the method for aluminium estimation in human albumin samples and should be used to control the limit of aluminium in human albumin blood products.","PeriodicalId":10889,"journal":{"name":"Current Pharmaceutical Analysis","volume":"1 1","pages":""},"PeriodicalIF":0.6,"publicationDate":"2024-09-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142181869","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-05DOI: 10.2174/0115734129317679240829055442
Qiang Sun, Ruinian Tong, Pengcheng Fan, Yiqing Li, Yu Wang, Feng Fang, Xionghua Jin, Min Zhang, Run Lei, Steven Xu
Background: Atypical peaks were observed in capillary electrophoresis with sodium dodecyl sulfate (CE-SDS) during the development of therapeutic monoclonal IgG4 antibodies (mAb-X). Based on the previous literature reports, the atypical peak may be caused by various factors such as post-translational modifications (PTMs), method-induced artifacts, sample degradation and sequence variants. Due to the high complexity structure of mAbs and the limitations of CE-SDS, acquiring comprehensive profiling of atypical peaks has historically been challenging. Objective: Here we developed a strategy utilizing complementary analytical methods to identify the cause of atypical peak. Methods: This strategy includes optimizing reduced CE-SDS method to evaluate artifacts induced by the analytical method, excluding potential glycation modifications, and utilizing Liquid Chromatograph Mass Spectrometer (LC-MS) to characterize mAb-X. Results: Our study demonstrates that the atypical peaks of mAb-X are a mixture of method-induced artifacts and variants in the C-terminal extension sequence of the light chain. Conclusion: Strategy for complementary analytical methods tools helps to identify the cause of unknown species and plays a key role in product and process characterization.
{"title":"Identification of Method-Induced Artifacts and Light Chain C-terminal Extension Sequence Variants in Therapeutic Monoclonal Antibodies by Complementary Analytical Methods","authors":"Qiang Sun, Ruinian Tong, Pengcheng Fan, Yiqing Li, Yu Wang, Feng Fang, Xionghua Jin, Min Zhang, Run Lei, Steven Xu","doi":"10.2174/0115734129317679240829055442","DOIUrl":"https://doi.org/10.2174/0115734129317679240829055442","url":null,"abstract":"Background: Atypical peaks were observed in capillary electrophoresis with sodium dodecyl sulfate (CE-SDS) during the development of therapeutic monoclonal IgG4 antibodies (mAb-X). Based on the previous literature reports, the atypical peak may be caused by various factors such as post-translational modifications (PTMs), method-induced artifacts, sample degradation and sequence variants. Due to the high complexity structure of mAbs and the limitations of CE-SDS, acquiring comprehensive profiling of atypical peaks has historically been challenging. Objective: Here we developed a strategy utilizing complementary analytical methods to identify the cause of atypical peak. Methods: This strategy includes optimizing reduced CE-SDS method to evaluate artifacts induced by the analytical method, excluding potential glycation modifications, and utilizing Liquid Chromatograph Mass Spectrometer (LC-MS) to characterize mAb-X. Results: Our study demonstrates that the atypical peaks of mAb-X are a mixture of method-induced artifacts and variants in the C-terminal extension sequence of the light chain. Conclusion: Strategy for complementary analytical methods tools helps to identify the cause of unknown species and plays a key role in product and process characterization.","PeriodicalId":10889,"journal":{"name":"Current Pharmaceutical Analysis","volume":"3 1","pages":""},"PeriodicalIF":0.6,"publicationDate":"2024-09-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142181870","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-09-05DOI: 10.2174/0115734129329774240829073320
Samanwita Khanra, Parikshit Roychowdhury, Gowthamarajan Kuppusamy, Nihar Ranjan Bhuyan, Shanmugam Ramaswamy, Jeyaprakash M R
Background: Oxaliplatin, a platinum-based antineoplastic agent, is widely used to treat colorectal cancer. It is well-known for its capacity to hinder the development and division of cells, especially fast-dividing ones, like cancer cells, via the creation of DNA adduct. The currently published oxaliplatin analytical methods require a complex, difficult-to-understand procedure, and are costly. Objective: The main objectives of our study were to select the chromatographic parameters, develop a UFLC method and validate it, and validate the results according to ICH guidelines. Method: In this UFLC study, a normal phase C18 column (250cm x 4.6 mm x5 μm) with a mobile phase containing 0.01 M orthophosphoric acid and acetonitrile (95:5 V/V) has been used at pH 3.5. Flowrate has been fixed at 1ml/min and the sample has been tested in the UV range for detection. The methods have been validated for precision, linearity, forced degradation studies, robustness, and accuracy. Results: The retention time of the drug has been found to be >8min. The calibration curve of the drug has been obtained within the range of 10–240 μg/ml. The results of this analysis have been validated according to ICH guideline Q2 (R1) for registration of human use. Conclusion: The UFLC method we have used for oxaliplatin quantification has been found to be simpler, easier to understand, and more cost-effective than standard HPLC as it has consumed less mobile phase and less time. Thus, we can conclude that this new, simple, and easy method may be a useful alternative to the existing standard methods for oxaliplatin.
背景：奥沙利铂是一种铂类抗肿瘤药物，被广泛用于治疗结直肠癌。众所周知，奥沙利铂能通过生成 DNA 加合物阻碍细胞（尤其是癌细胞等快速分裂的细胞）的发育和分裂。目前公布的奥沙利铂分析方法需要复杂、难以理解的程序，而且成本高昂。研究目的我们研究的主要目的是选择色谱参数、开发超高效液相色谱法并进行验证，以及根据 ICH 指南验证结果。方法：在这项超高效液相色谱研究中，使用了正相 C18 色谱柱（250 厘米 x 4.6 毫米 x 5 微米），流动相为 0.01 M 正磷酸和乙腈（95:5 V/V），pH 值为 3.5。流速固定为 1 毫升/分钟，样品在紫外检测范围内进行检测。该方法已通过精密度、线性、强制降解研究、稳健性和准确性验证。结果：药物的保留时间为 8 分钟。药物的校准曲线范围为 10-240 μg/ml。该分析结果已根据 ICH 指南 Q2 (R1) 进行了人体使用注册验证。结论与标准高效液相色谱法相比，我们所采用的超高效液相色谱法用于奥沙利铂的定量分析，不仅操作简单、易于理解，而且成本效益更高，因为它所消耗的流动相和时间更少。因此，我们可以得出结论，这种简单易行的新方法可以替代现有的奥沙利铂标准方法。
{"title":"Development and Validation of an RP-UFLC Method for the Estimation of Oxaliplatin Drug for the Preparation of Oxaliplatin Nanoparticles","authors":"Samanwita Khanra, Parikshit Roychowdhury, Gowthamarajan Kuppusamy, Nihar Ranjan Bhuyan, Shanmugam Ramaswamy, Jeyaprakash M R","doi":"10.2174/0115734129329774240829073320","DOIUrl":"https://doi.org/10.2174/0115734129329774240829073320","url":null,"abstract":"Background: Oxaliplatin, a platinum-based antineoplastic agent, is widely used to treat colorectal cancer. It is well-known for its capacity to hinder the development and division of cells, especially fast-dividing ones, like cancer cells, via the creation of DNA adduct. The currently published oxaliplatin analytical methods require a complex, difficult-to-understand procedure, and are costly. Objective: The main objectives of our study were to select the chromatographic parameters, develop a UFLC method and validate it, and validate the results according to ICH guidelines. Method: In this UFLC study, a normal phase C18 column (250cm x 4.6 mm x5 μm) with a mobile phase containing 0.01 M orthophosphoric acid and acetonitrile (95:5 V/V) has been used at pH 3.5. Flowrate has been fixed at 1ml/min and the sample has been tested in the UV range for detection. The methods have been validated for precision, linearity, forced degradation studies, robustness, and accuracy. Results: The retention time of the drug has been found to be >8min. The calibration curve of the drug has been obtained within the range of 10–240 μg/ml. The results of this analysis have been validated according to ICH guideline Q2 (R1) for registration of human use. Conclusion: The UFLC method we have used for oxaliplatin quantification has been found to be simpler, easier to understand, and more cost-effective than standard HPLC as it has consumed less mobile phase and less time. Thus, we can conclude that this new, simple, and easy method may be a useful alternative to the existing standard methods for oxaliplatin.","PeriodicalId":10889,"journal":{"name":"Current Pharmaceutical Analysis","volume":"22 1","pages":""},"PeriodicalIF":0.6,"publicationDate":"2024-09-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142181871","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Purpose: A simple, rapid and precise reverse phase–High performance liquid chromatography (RP-HPLC) method was developed for the determination of degradation impurity i.e. Oxidised follitropin in recombinant Follicle Stimulating Hormone (rFSH) Injection. Methods: Chromatographic separation was performed using a C4 column of size: 250 × 4.6 mm, 5 μm along with C3 Guard Column (SB-C3 size: 125 mm x 4.6 mm, 5 μm) and using gradient elution. The flow rate was kept at 1.0 ml per minute and the detection wavelength was at 210 nm. The retention time of oxidised follitropin was ~14 to 15 minutes. The detector showed a linear response between the range of 2.46–63.325 μg/ml (5% - 125%) with a correlation coefficient value of 0.9987. After establishing the procedure, it was ensured for its intended usage by validation of the analytical parameters like specificity, linearity, accuracy, repeatability, and robustness as per the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) [Q2 (R1) Validation of Analytical Procedures: Text and Methodology]. Results: All of the parameters performed using the current method yielded results that met the acceptance requirements. The detector showed a linear response between the range of 2.46– 63.325 μg/ml (5% - 125%) with a correlation coefficient value of 0.9987. Conclusions: As a result, a newly designed RP-HPLC method was capable of effectively separating impurities while maintaining acceptable limits.
{"title":"Analytical Method Development and Validation to Determine Oxidized Follitropin Recombinant Follicle Stimulating Hormone (rFSH) Injection by RP-HPLC","authors":"Priyanka Chaudhary, Muthusamy Kalaivani, Pavisha Tyagi, Anubhuti Goyal, Meenakshi Dahiya, Rajeev Singh Raghuvanshi","doi":"10.2174/0115734129316027240830074632","DOIUrl":"https://doi.org/10.2174/0115734129316027240830074632","url":null,"abstract":"Purpose: A simple, rapid and precise reverse phase–High performance liquid chromatography (RP-HPLC) method was developed for the determination of degradation impurity i.e. Oxidised follitropin in recombinant Follicle Stimulating Hormone (rFSH) Injection. Methods: Chromatographic separation was performed using a C4 column of size: 250 × 4.6 mm, 5 μm along with C3 Guard Column (SB-C3 size: 125 mm x 4.6 mm, 5 μm) and using gradient elution. The flow rate was kept at 1.0 ml per minute and the detection wavelength was at 210 nm. The retention time of oxidised follitropin was ~14 to 15 minutes. The detector showed a linear response between the range of 2.46–63.325 μg/ml (5% - 125%) with a correlation coefficient value of 0.9987. After establishing the procedure, it was ensured for its intended usage by validation of the analytical parameters like specificity, linearity, accuracy, repeatability, and robustness as per the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) [Q2 (R1) Validation of Analytical Procedures: Text and Methodology]. Results: All of the parameters performed using the current method yielded results that met the acceptance requirements. The detector showed a linear response between the range of 2.46– 63.325 μg/ml (5% - 125%) with a correlation coefficient value of 0.9987. Conclusions: As a result, a newly designed RP-HPLC method was capable of effectively separating impurities while maintaining acceptable limits.","PeriodicalId":10889,"journal":{"name":"Current Pharmaceutical Analysis","volume":"30 1","pages":""},"PeriodicalIF":0.6,"publicationDate":"2024-09-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142181873","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-08-29DOI: 10.2174/0115734129300505240813055500
Sun Yan Ni, Ai Yun, Wang Jin Rui, He Ying, Zhang Lu, Tian Bin Bin, Tao Shun Peng, Liu Jian Li, Zhang Ning
Background: Radix astragali (a Tonic-Qi traditional Chinese medicine) can enhance cellular metabolism and increase the life span of cells. Spermidine can markedly extend the lifespan. On the basis of these considerations, we assumed whether any relationship existed between the anti-aging activity of Radix astragali and spermidine. Methods: In this research, spermidine and 10 other kinds of Biogenic amines in Radix astragali samples were identified and determined using High-Performance Liquid Chromatography-Diode Array Detector (HPLC-DAD) with precolumn derivatization. Biogenic amines were extracted with hydrochloric acid, purified by n-butyl alcohol-dichloromethane extraction, and reacted with dansyl chloride for derivatization before HPLC analysis. Results: The method had good repeatability and reproducibility for the quantitative determination of biogenic amines in Radix astragali samples. Putrescine, spermidine, and spermine were detected in 10 batches of Radix astragali samples. The total Biogenic amines concentration was 48.09±2.22 mg/kg. Spermidine (22.84±2.59 mg/kg) was the highest amine in Radix astragali samples, followed by putrescine and spermine. This is the first report that suggests that Radix astragali contains Biogenic amines, especially high-content spermidine. Conclusion: The high content of spermidine might be the one reason for Radix astragali with Tonic- Qi and anti-aging effect.
{"title":"Determination of Spermidine and other 10 Biogenic Amines in Radix astragali (Huang qi) by HPLC-DAD with Precolumn Derivatization","authors":"Sun Yan Ni, Ai Yun, Wang Jin Rui, He Ying, Zhang Lu, Tian Bin Bin, Tao Shun Peng, Liu Jian Li, Zhang Ning","doi":"10.2174/0115734129300505240813055500","DOIUrl":"https://doi.org/10.2174/0115734129300505240813055500","url":null,"abstract":"Background: Radix astragali (a Tonic-Qi traditional Chinese medicine) can enhance cellular metabolism and increase the life span of cells. Spermidine can markedly extend the lifespan. On the basis of these considerations, we assumed whether any relationship existed between the anti-aging activity of Radix astragali and spermidine. Methods: In this research, spermidine and 10 other kinds of Biogenic amines in Radix astragali samples were identified and determined using High-Performance Liquid Chromatography-Diode Array Detector (HPLC-DAD) with precolumn derivatization. Biogenic amines were extracted with hydrochloric acid, purified by n-butyl alcohol-dichloromethane extraction, and reacted with dansyl chloride for derivatization before HPLC analysis. Results: The method had good repeatability and reproducibility for the quantitative determination of biogenic amines in Radix astragali samples. Putrescine, spermidine, and spermine were detected in 10 batches of Radix astragali samples. The total Biogenic amines concentration was 48.09±2.22 mg/kg. Spermidine (22.84±2.59 mg/kg) was the highest amine in Radix astragali samples, followed by putrescine and spermine. This is the first report that suggests that Radix astragali contains Biogenic amines, especially high-content spermidine. Conclusion: The high content of spermidine might be the one reason for Radix astragali with Tonic- Qi and anti-aging effect.","PeriodicalId":10889,"journal":{"name":"Current Pharmaceutical Analysis","volume":"59 1","pages":""},"PeriodicalIF":0.6,"publicationDate":"2024-08-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142181894","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-08-29DOI: 10.2174/0115734129322567240821052326
Chandni V. Chandarana, Namira T. Mithani, Diksha V. Singh, Utkarsh B. Kikani
Introduction: Infrared and Raman spectroscopy have emerged as promising diagnostic tools for gastric and liver cancer, offering significant advantages over traditional histology and biomarker- based methods. Methods: These spectroscopic techniques provide rapid and highly specific molecular fingerprinting with minimal sample preparation, enabling real-time diagnosis and preserving samples for further analysis. The integration of nanoparticles, particularly in surface-enhanced Raman spectroscopy, enhances the sensitivity and resolution of the method by amplifying signal strengths through localized surface plasmon resonances. This advancement facilitates the detection of subtle molecular changes associated with cancer, even at early stages. Results: Raman spectroscopy, a non-destructive technique, can differentiate between healthy and malignant cells, aiding in the diagnosis of various gastric cancer forms, including adenocarcinoma and gastrointestinal stromal tumors. Similarly, IR spectroscopy provides insights into the chemical composition of tissues, detecting molecular changes associated with cancer. For liver cancer, including hepatocellular carcinoma, these spectroscopic methods reveal biochemical alterations, facilitating early detection and characterization of the disease. This review explores the application of Raman and IR spectroscopy in diagnosing gastric and liver cancers, emphasizing their potential to enhance diagnostic accuracy and improve patient outcomes by identifying molecular changes linked to malignancies. Conclusion: Overall, the integration of nanoparticles into spectroscopic techniques holds significant potential for improving the accuracy, speed, and efficacy of cancer diagnostics.
{"title":"Vibrational Spectrophotometry: A Comprehensive Review on the Diagnosis of Gastric and Liver Cancer","authors":"Chandni V. Chandarana, Namira T. Mithani, Diksha V. Singh, Utkarsh B. Kikani","doi":"10.2174/0115734129322567240821052326","DOIUrl":"https://doi.org/10.2174/0115734129322567240821052326","url":null,"abstract":"Introduction: Infrared and Raman spectroscopy have emerged as promising diagnostic tools for gastric and liver cancer, offering significant advantages over traditional histology and biomarker- based methods. Methods: These spectroscopic techniques provide rapid and highly specific molecular fingerprinting with minimal sample preparation, enabling real-time diagnosis and preserving samples for further analysis. The integration of nanoparticles, particularly in surface-enhanced Raman spectroscopy, enhances the sensitivity and resolution of the method by amplifying signal strengths through localized surface plasmon resonances. This advancement facilitates the detection of subtle molecular changes associated with cancer, even at early stages. Results: Raman spectroscopy, a non-destructive technique, can differentiate between healthy and malignant cells, aiding in the diagnosis of various gastric cancer forms, including adenocarcinoma and gastrointestinal stromal tumors. Similarly, IR spectroscopy provides insights into the chemical composition of tissues, detecting molecular changes associated with cancer. For liver cancer, including hepatocellular carcinoma, these spectroscopic methods reveal biochemical alterations, facilitating early detection and characterization of the disease. This review explores the application of Raman and IR spectroscopy in diagnosing gastric and liver cancers, emphasizing their potential to enhance diagnostic accuracy and improve patient outcomes by identifying molecular changes linked to malignancies. Conclusion: Overall, the integration of nanoparticles into spectroscopic techniques holds significant potential for improving the accuracy, speed, and efficacy of cancer diagnostics.","PeriodicalId":10889,"journal":{"name":"Current Pharmaceutical Analysis","volume":"12 1","pages":""},"PeriodicalIF":0.6,"publicationDate":"2024-08-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142181874","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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