Abstract The inherent complexity of the human biological matrix and its importance in modern medical diagnosis and medical research promote the development of modern analytical technology. Solid-phase microextraction technology has been widely used in the treatment and analysis of different complex biological matrices due to its smaller sample size, simpler sample preparation and setting, and lower consumption of harmful chemicals. This review provides updated information on headspace solid-phase microextraction combined with gas chromatography technique applications, focusing on the analysis of volatile and semivolatile compounds in human biological matrices. The application of headspace solid-phase microextraction combined with gas chromatography techniques in human biological matrix analysis is mainly summarized into three aspects, namely, to discover biomarkers, to investigate volatile metabolomics, and to explore the effect of the external environment on volatile metabolomics of the human biological matrix. In addition, the frequently used statistical analytical methods are summarized, and the application prospect of solid-phase microextraction in the analysis of human biological matrices is proposed.
{"title":"Applications of headspace solid-phase microextraction in human biological matrix analysis","authors":"X. Ji","doi":"10.1515/revac-2022-0042","DOIUrl":"https://doi.org/10.1515/revac-2022-0042","url":null,"abstract":"Abstract The inherent complexity of the human biological matrix and its importance in modern medical diagnosis and medical research promote the development of modern analytical technology. Solid-phase microextraction technology has been widely used in the treatment and analysis of different complex biological matrices due to its smaller sample size, simpler sample preparation and setting, and lower consumption of harmful chemicals. This review provides updated information on headspace solid-phase microextraction combined with gas chromatography technique applications, focusing on the analysis of volatile and semivolatile compounds in human biological matrices. The application of headspace solid-phase microextraction combined with gas chromatography techniques in human biological matrix analysis is mainly summarized into three aspects, namely, to discover biomarkers, to investigate volatile metabolomics, and to explore the effect of the external environment on volatile metabolomics of the human biological matrix. In addition, the frequently used statistical analytical methods are summarized, and the application prospect of solid-phase microextraction in the analysis of human biological matrices is proposed.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":4.3,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82394960","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract In this work, spectrophotometric identification of acetylsalicylic acid (ASA), paracetamol (PCM), and caffeine (CAF) (common cold infection drugs) in human urine samples was investigated. For ASA, PCM, and CAF, chemometric analysis of human urine samples has proved successful. Spectrophotometric analysis of common cold infection drugs was performed using multivariate calibration methods (principal component regression [PCR] and partial least-squares regression). For the simultaneous prediction of common cold infection drugs in prepared mixes and human urine samples without prior separation, two spectrophotometric-chemometric approaches were proposed. The synthetic mixes were made with common cold infection drugs in the first stage, and the absorbance values were obtained using spectrophotometry. The quantities of common cold infection drugs in the human urine sample were calculated in the second stage. The calibration curves for each medication are linear in the concentration range of the synthetic mixes. The two methods were tested for accuracy and repeatability, and high recoveries and low standard deviations were calculated. sum of prediction residual errors, observation limit, and detection limit, and % recovery values, which are the analytical properties of the proposed methods, were 0.00029, 0.096, and 0.290, respectively; 0.0069, 0.086, and 0.260; 0.0077, 0.094, and 0.285; 0.0049, 0.066, and 0.199 for PCM, ASA, and CAF for the principal component regression method, respectively; 0.0059, 0.066, and 0.199; 0.0065, 0.069, and 0.210. The results produced using the employed chemometric methods are quick, easy, and consistent. The proposed methods are extremely sensitive and precise and have thus been effectively employed to detect active chemicals (ASA, PCM, and CAF) in human urine samples.
{"title":"Chemometric determination of common cold infection drugs in human urine","authors":"G. Ertokus","doi":"10.1515/revac-2022-0040","DOIUrl":"https://doi.org/10.1515/revac-2022-0040","url":null,"abstract":"Abstract In this work, spectrophotometric identification of acetylsalicylic acid (ASA), paracetamol (PCM), and caffeine (CAF) (common cold infection drugs) in human urine samples was investigated. For ASA, PCM, and CAF, chemometric analysis of human urine samples has proved successful. Spectrophotometric analysis of common cold infection drugs was performed using multivariate calibration methods (principal component regression [PCR] and partial least-squares regression). For the simultaneous prediction of common cold infection drugs in prepared mixes and human urine samples without prior separation, two spectrophotometric-chemometric approaches were proposed. The synthetic mixes were made with common cold infection drugs in the first stage, and the absorbance values were obtained using spectrophotometry. The quantities of common cold infection drugs in the human urine sample were calculated in the second stage. The calibration curves for each medication are linear in the concentration range of the synthetic mixes. The two methods were tested for accuracy and repeatability, and high recoveries and low standard deviations were calculated. sum of prediction residual errors, observation limit, and detection limit, and % recovery values, which are the analytical properties of the proposed methods, were 0.00029, 0.096, and 0.290, respectively; 0.0069, 0.086, and 0.260; 0.0077, 0.094, and 0.285; 0.0049, 0.066, and 0.199 for PCM, ASA, and CAF for the principal component regression method, respectively; 0.0059, 0.066, and 0.199; 0.0065, 0.069, and 0.210. The results produced using the employed chemometric methods are quick, easy, and consistent. The proposed methods are extremely sensitive and precise and have thus been effectively employed to detect active chemicals (ASA, PCM, and CAF) in human urine samples.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":4.3,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88053614","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract Analysis of complex samples in environmental matrices poses extreme challenge for analytical chemists as the number of known and unknown compounds are numerous and have varying physical and chemical properties. The introduction, over the past decade, of comprehensive two-dimensional (2D) gas chromatography (GC × GC) paired with mass spectrometry (MS) has tremendously changed the analytical profiles of ultra-trace levels of organic pollutants from different environmental media. This review article provides a summary of selected articles using comprehensive 2D GC/MS-based methodologies from January 2014 to August 2019. The applications of various MS detectors, such as single (Q) and triple (QqQ) quadrupole, low resolution and high resolution time-of-flight (TOF), and the hybrid (quadrupole TOF-MS), coupled to GC × GC, and their benefits for analyzing persistent and emerging organic pollutants when applied to different environmental matrices were discussed. Emphasis was given to reviewing some applications of GC × GC-electron capture detector (ECD) and GC × GC-μECD within the specified period as these detectors have improved selectivity and sensitivity toward halogenated (bromine and chloride) compounds found in ultra-trace levels of environmental media.
{"title":"A review of the application of comprehensive two-dimensional gas chromatography MS-based techniques for the analysis of persistent organic pollutants and ultra-trace level of organic pollutants in environmental samples","authors":"Oliver Vaye, R. S. Ngumbu, Dan Xia","doi":"10.1515/revac-2022-0034","DOIUrl":"https://doi.org/10.1515/revac-2022-0034","url":null,"abstract":"Abstract Analysis of complex samples in environmental matrices poses extreme challenge for analytical chemists as the number of known and unknown compounds are numerous and have varying physical and chemical properties. The introduction, over the past decade, of comprehensive two-dimensional (2D) gas chromatography (GC × GC) paired with mass spectrometry (MS) has tremendously changed the analytical profiles of ultra-trace levels of organic pollutants from different environmental media. This review article provides a summary of selected articles using comprehensive 2D GC/MS-based methodologies from January 2014 to August 2019. The applications of various MS detectors, such as single (Q) and triple (QqQ) quadrupole, low resolution and high resolution time-of-flight (TOF), and the hybrid (quadrupole TOF-MS), coupled to GC × GC, and their benefits for analyzing persistent and emerging organic pollutants when applied to different environmental matrices were discussed. Emphasis was given to reviewing some applications of GC × GC-electron capture detector (ECD) and GC × GC-μECD within the specified period as these detectors have improved selectivity and sensitivity toward halogenated (bromine and chloride) compounds found in ultra-trace levels of environmental media.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":4.3,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84268234","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
S. Cho, Van-An Duong, Jeong-Hun Mok, MinJoong Joo, Jong-Moon Park, Hookeun Lee
Abstract Glycation is a spontaneous post-translational modification of lysine, arginine, and the N-terminus of proteins. Protein glycation is closely related to the pathogenesis of human diseases, including diabetes, Alzheimer’s disease, renal disease, and cancer. The levels of advanced glycation end products (AGEs) are positively correlated with the progression of many diseases. However, it remains challenging to analyze glycation-related products, such as reactive carbonyl species, Schiff bases, Amadori compounds, and AGEs, because of their high heterogeneity. Many analysis methods, such as fluorescence detection, immunoassays, and liquid chromatography-tandem mass spectrometry, have attempted to correlate glycation products with diseases. Some enrichment methods have been used to increase the probability of detection of glycated proteins due to their low abundance in blood plasma. This review summarizes the enrichment and analysis methods that are currently used to identify glycation as a disease biomarker in exploratory studies.
{"title":"Enrichment and analysis of glycated proteins","authors":"S. Cho, Van-An Duong, Jeong-Hun Mok, MinJoong Joo, Jong-Moon Park, Hookeun Lee","doi":"10.1515/revac-2022-0036","DOIUrl":"https://doi.org/10.1515/revac-2022-0036","url":null,"abstract":"Abstract Glycation is a spontaneous post-translational modification of lysine, arginine, and the N-terminus of proteins. Protein glycation is closely related to the pathogenesis of human diseases, including diabetes, Alzheimer’s disease, renal disease, and cancer. The levels of advanced glycation end products (AGEs) are positively correlated with the progression of many diseases. However, it remains challenging to analyze glycation-related products, such as reactive carbonyl species, Schiff bases, Amadori compounds, and AGEs, because of their high heterogeneity. Many analysis methods, such as fluorescence detection, immunoassays, and liquid chromatography-tandem mass spectrometry, have attempted to correlate glycation products with diseases. Some enrichment methods have been used to increase the probability of detection of glycated proteins due to their low abundance in blood plasma. This review summarizes the enrichment and analysis methods that are currently used to identify glycation as a disease biomarker in exploratory studies.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":4.3,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84682235","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Khairi Mustafa Salem Fahelelbom, A. Saleh, M. Al-Tabakha, A. Ashames
Abstract Qualitative Fourier transform infrared (FTIR) spectroscopy has long been established and implemented in a wide variety of fields including pharmaceutical, biomedical, and clinical fields. While the quantitative applications are yet to reach their full potential, this technique is flourishing. It is tempting to shed light on modern engaging and the applicability of analytical quantitative FTIR spectroscopy in the aforementioned fields. More importantly, the credibility, validity, and generality of the application will be thoroughly demonstrated by reviewing the latest published work in the scientific literature. Utilizing FTIR spectroscopy in a quantitative approach in pharmaceutical, biomedical, and interdisciplinary fields has many undeniable advantages over traditional procedures. An insightful account will be undertaken in this regard. The technique will be introduced as an appealing alternative to common methods such as high performance liquid chromatography. It is anticipated that the review will offer researchers an update of the current status and prospect on the subject among the pharmacy and biomedical sciences both in academic and industrial fields.
{"title":"Recent applications of quantitative analytical FTIR spectroscopy in pharmaceutical, biomedical, and clinical fields: A brief review","authors":"Khairi Mustafa Salem Fahelelbom, A. Saleh, M. Al-Tabakha, A. Ashames","doi":"10.1515/revac-2022-0030","DOIUrl":"https://doi.org/10.1515/revac-2022-0030","url":null,"abstract":"Abstract Qualitative Fourier transform infrared (FTIR) spectroscopy has long been established and implemented in a wide variety of fields including pharmaceutical, biomedical, and clinical fields. While the quantitative applications are yet to reach their full potential, this technique is flourishing. It is tempting to shed light on modern engaging and the applicability of analytical quantitative FTIR spectroscopy in the aforementioned fields. More importantly, the credibility, validity, and generality of the application will be thoroughly demonstrated by reviewing the latest published work in the scientific literature. Utilizing FTIR spectroscopy in a quantitative approach in pharmaceutical, biomedical, and interdisciplinary fields has many undeniable advantages over traditional procedures. An insightful account will be undertaken in this regard. The technique will be introduced as an appealing alternative to common methods such as high performance liquid chromatography. It is anticipated that the review will offer researchers an update of the current status and prospect on the subject among the pharmacy and biomedical sciences both in academic and industrial fields.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":4.3,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81243820","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Andrea Dandic, Katarina Rajkovača, Marija Jozanović, Iva Pukles, A. Széchenyi, Mateja Budetić, Mirela Samardžić
Abstract Nonsteroidal anti-inflammatory drugs (NSAIDs) are the first choice of treatment for rheumatic disorders and other degenerative inflammatory diseases. One of them, indomethacin (INDO), is highlighted in this study. With its analgesic, antipyretic, and anti-inflammatory properties, it is one of the most powerful drugs used in various clinical trials and therapies related to the mechanism of blocking prostaglandin synthesis, thus reducing and eliminating many inflammatory conditions in patients. To ensure the efficacy and safety of this drug in pharmaceutical and clinical use, precise product quality control is required. Such control is performed with routine pharmaceutical analysis using various chemical methods by which INDO is identified as a separate active ingredient in the multicomponent system of a complete pharmaceutical form. In addition, the determination of INDO is important in clinical practice, where its concentration is determined in different biological samples, ensuring better monitoring of a particular therapy. The most commonly used methods for the determination of INDO are high-performance liquid chromatography (37% of developed methods), voltammetry (16% of developed methods), and UV spectroscopy (11% of developed methods). However, each of these methods must provide precise validation parameters. A combination of analytical methods can lead to more precise results and safer application in practice.
{"title":"Review of characteristics and analytical methods for determination of indomethacin","authors":"Andrea Dandic, Katarina Rajkovača, Marija Jozanović, Iva Pukles, A. Széchenyi, Mateja Budetić, Mirela Samardžić","doi":"10.1515/revac-2022-0032","DOIUrl":"https://doi.org/10.1515/revac-2022-0032","url":null,"abstract":"Abstract Nonsteroidal anti-inflammatory drugs (NSAIDs) are the first choice of treatment for rheumatic disorders and other degenerative inflammatory diseases. One of them, indomethacin (INDO), is highlighted in this study. With its analgesic, antipyretic, and anti-inflammatory properties, it is one of the most powerful drugs used in various clinical trials and therapies related to the mechanism of blocking prostaglandin synthesis, thus reducing and eliminating many inflammatory conditions in patients. To ensure the efficacy and safety of this drug in pharmaceutical and clinical use, precise product quality control is required. Such control is performed with routine pharmaceutical analysis using various chemical methods by which INDO is identified as a separate active ingredient in the multicomponent system of a complete pharmaceutical form. In addition, the determination of INDO is important in clinical practice, where its concentration is determined in different biological samples, ensuring better monitoring of a particular therapy. The most commonly used methods for the determination of INDO are high-performance liquid chromatography (37% of developed methods), voltammetry (16% of developed methods), and UV spectroscopy (11% of developed methods). However, each of these methods must provide precise validation parameters. A combination of analytical methods can lead to more precise results and safer application in practice.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":4.3,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83968631","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract During the production process of some copper clad laminate (CCL), the content of 3,3,5,7,7-pentamethyl-1,2,4-trioxepane in prepreg can affect the cross-linking and curing degree of resin directly, and thereby affect the properties of CCL. In this article, near-infrared (NIR) spectroscopy combined with partial least square regression using high performance liquid chromatography as a reference method were used for the determination of 3,3,5,7,7-pentamethyl-1,2,4-trioxepane in the CCL production progress. 160 spectra of prepreg samples randomly formed the calibration set, and 50 spectra of prepreg samples formed the validation set. The value of the root mean square error of calibration (w/w) and root mean square error of prediction (w/w) were 0.011% and 0.013% for 3,3,5,7,7-pentamethyl-1,2,4-trioxepane content (%, w/w), and the calculation and validation of the regression equation resulted in high correlation coefficients of 0.99 and 0.98, respectively. The scatter plot value of calibration set which was obtained from the root mean square error of cross-validation (w/w) was 0.015%, and the regression equation resulted in high correlation coefficient of 0.98. The results of the paired t-test revealed that there was no significant difference between NIR and HPLC method. Thus, the results obtained in this study reflect that NIR could be used as a rapid, accurate, and simultaneous technique to determine 3,3,5,7,7-pentamethyl-1,2,4-trioxepane content of prepreg in the production process.
{"title":"Analysis of initiator content of prepreg by near-infrared spectroscopy","authors":"Qian Liu, Dan Li, Chiji Guan","doi":"10.1515/revac-2022-0035","DOIUrl":"https://doi.org/10.1515/revac-2022-0035","url":null,"abstract":"Abstract During the production process of some copper clad laminate (CCL), the content of 3,3,5,7,7-pentamethyl-1,2,4-trioxepane in prepreg can affect the cross-linking and curing degree of resin directly, and thereby affect the properties of CCL. In this article, near-infrared (NIR) spectroscopy combined with partial least square regression using high performance liquid chromatography as a reference method were used for the determination of 3,3,5,7,7-pentamethyl-1,2,4-trioxepane in the CCL production progress. 160 spectra of prepreg samples randomly formed the calibration set, and 50 spectra of prepreg samples formed the validation set. The value of the root mean square error of calibration (w/w) and root mean square error of prediction (w/w) were 0.011% and 0.013% for 3,3,5,7,7-pentamethyl-1,2,4-trioxepane content (%, w/w), and the calculation and validation of the regression equation resulted in high correlation coefficients of 0.99 and 0.98, respectively. The scatter plot value of calibration set which was obtained from the root mean square error of cross-validation (w/w) was 0.015%, and the regression equation resulted in high correlation coefficient of 0.98. The results of the paired t-test revealed that there was no significant difference between NIR and HPLC method. Thus, the results obtained in this study reflect that NIR could be used as a rapid, accurate, and simultaneous technique to determine 3,3,5,7,7-pentamethyl-1,2,4-trioxepane content of prepreg in the production process.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":4.3,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75283778","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract Ibrutinib is a drug used for the treatment of marginal zone lymphoma, mantle cell lymphoma, lymphocytic leukemia, chronic graft, and Waldenstrom macroglobulinemia. A simple, sensitive, and fast liquid chromatographic and spectrophotometric method for the quantification of ibrutinib in pharmaceutical forms and bulk was developed and validated. The chromatographic technique was developed using an ODS 3 C 18 (250 mm × 4.6 mm i.d., 5 µm) column. The mobile phase was a mixture of 0.1% trifluoroacetic acid in water and acetonitrile (50/50, v/v) at a flow rate of 1.0 mL·min−1. Eluent detection was carried out at a wavelength of 260 nm using a ultraviolet detector. The retention time of ibrutinib was found to be 5.27. On the other hand, Ibrutinib was determined using a spectrophotometric technique by measuring the absorbance of the solutions at a wavelength of 260 nm. The developed techniques were validated in accordance with the protocols outlined in International conference on harmonisation of technical requirements for registration of pharmaceuticals for human (ICH) guidelines Q2(R1). Correlation coefficients for both methods were greater than 0.999 in the concentration range of 5–30 mg·mL−1. The relative standard deviation values were low in intraday and interday precision tests. The accuracy of the developed techniques ranged 99.74–100.23% for the chromatographic method and 99.32–100.76% for the spectrophotometric method. The limits of detection and quantitation were 0.90 and 2.80 µg·mL−1 for the chromatographic method and 1.10 and 3.20 µg·mL−1 for the spectrophotometric method. The developed and validated analytical methods can be safely used in quality control tests for the determination of the amount of ibrutinib in pharmaceutical products.
伊鲁替尼是一种用于治疗边缘带淋巴瘤、套细胞淋巴瘤、淋巴细胞白血病、慢性移植物和Waldenstrom巨球蛋白血症的药物。建立了一种简便、灵敏、快速的液相色谱和分光光度法定量测定依鲁替尼制剂和散装制剂的方法。色谱技术采用ODS 3c 18 (250 mm × 4.6 mm, 5µm)色谱柱。流动相为0.1%三氟乙酸水溶液与乙腈(50/50,v/v)的混合物，流速为1.0 mL·min−1。用紫外检测器在波长260 nm处对洗脱液进行检测。依鲁替尼的保留时间为5.27。另一方面，通过测量溶液在260 nm波长处的吸光度，采用分光光度法测定伊鲁替尼。所开发的技术根据国际人用药品注册技术要求协调会议(ICH)指南Q2(R1)中概述的协议进行了验证。在5 ~ 30 mg·mL−1浓度范围内，两种方法的相关系数均大于0.999。日间和日间精密度试验的相对标准偏差值较低。色谱法的准确度为99.74 ~ 100.23%，分光光度法的准确度为99.32 ~ 100.76%。色谱法的检出限和定量限分别为0.90和2.80µg·mL−1，分光光度法的检出限和定量限分别为1.10和3.20µg·mL−1。开发和验证的分析方法可以安全地用于质量控制测试，以确定药品中伊鲁替尼的含量。
{"title":"Alternative analytical methods for ibrutinib quantification in pharmaceutical formulation: A statistical comparison","authors":"Erten Akbel, S. Güngör, I. Bulduk","doi":"10.1515/revac-2022-0039","DOIUrl":"https://doi.org/10.1515/revac-2022-0039","url":null,"abstract":"Abstract Ibrutinib is a drug used for the treatment of marginal zone lymphoma, mantle cell lymphoma, lymphocytic leukemia, chronic graft, and Waldenstrom macroglobulinemia. A simple, sensitive, and fast liquid chromatographic and spectrophotometric method for the quantification of ibrutinib in pharmaceutical forms and bulk was developed and validated. The chromatographic technique was developed using an ODS 3 C 18 (250 mm × 4.6 mm i.d., 5 µm) column. The mobile phase was a mixture of 0.1% trifluoroacetic acid in water and acetonitrile (50/50, v/v) at a flow rate of 1.0 mL·min−1. Eluent detection was carried out at a wavelength of 260 nm using a ultraviolet detector. The retention time of ibrutinib was found to be 5.27. On the other hand, Ibrutinib was determined using a spectrophotometric technique by measuring the absorbance of the solutions at a wavelength of 260 nm. The developed techniques were validated in accordance with the protocols outlined in International conference on harmonisation of technical requirements for registration of pharmaceuticals for human (ICH) guidelines Q2(R1). Correlation coefficients for both methods were greater than 0.999 in the concentration range of 5–30 mg·mL−1. The relative standard deviation values were low in intraday and interday precision tests. The accuracy of the developed techniques ranged 99.74–100.23% for the chromatographic method and 99.32–100.76% for the spectrophotometric method. The limits of detection and quantitation were 0.90 and 2.80 µg·mL−1 for the chromatographic method and 1.10 and 3.20 µg·mL−1 for the spectrophotometric method. The developed and validated analytical methods can be safely used in quality control tests for the determination of the amount of ibrutinib in pharmaceutical products.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":4.3,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78882555","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract An improved management of secondary raw materials (SRM) is a crucial contribution for a circular economy and necessitates knowledge about the composition of wastes and SRM. However, this information is scarce and has to be determined with chemical analysis (CA). CA of SRM faces challenges, which can be approached by using round robin tests (RRT) to identify deviations from the “true value” of an element/molecule content. An RRT is a testing approach, which involves multiple labs to analyze one or more samples and evaluates the lab results with regard to the goal of the RRT. This article presents a systematic literature review and investigates which purposes and which performance parameters (PP) are commonly applied in RRT of SRM. The examined literature shows that the two main purposes applied are assessment of method performance and assessment of lab performance. PP can be categorized into trueness performance parameters (TPP; assessing the deviation of a value from a reference value) and precision performance parameters (PPP; describing the variability of a data set). The main TPP identified are z score and relative deviation, the main PPP identified are standard deviation and relative standard deviation. These results offer the conclusions that RRT can be used as a bespoke method to deal with analytical effects and that the selection of PP for an RRT could be based on simplicity.
{"title":"Round robin tests of secondary raw materials: A systematic review of performance parameters","authors":"N. Korf, P. Mählitz, V. S. Rotter","doi":"10.1515/revac-2022-0033","DOIUrl":"https://doi.org/10.1515/revac-2022-0033","url":null,"abstract":"Abstract An improved management of secondary raw materials (SRM) is a crucial contribution for a circular economy and necessitates knowledge about the composition of wastes and SRM. However, this information is scarce and has to be determined with chemical analysis (CA). CA of SRM faces challenges, which can be approached by using round robin tests (RRT) to identify deviations from the “true value” of an element/molecule content. An RRT is a testing approach, which involves multiple labs to analyze one or more samples and evaluates the lab results with regard to the goal of the RRT. This article presents a systematic literature review and investigates which purposes and which performance parameters (PP) are commonly applied in RRT of SRM. The examined literature shows that the two main purposes applied are assessment of method performance and assessment of lab performance. PP can be categorized into trueness performance parameters (TPP; assessing the deviation of a value from a reference value) and precision performance parameters (PPP; describing the variability of a data set). The main TPP identified are z score and relative deviation, the main PPP identified are standard deviation and relative standard deviation. These results offer the conclusions that RRT can be used as a bespoke method to deal with analytical effects and that the selection of PP for an RRT could be based on simplicity.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":4.3,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"91322699","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abstract This study was designed to determine the 11 metal elements (Al, Cr, Mn, Fe, As, Ni, Cu, Zn, Cd, Sb, and Pb) in soy sauce and their migration from the containing glass bottles. Inductively coupled plasma mass spectrometry (ICP-MS) was applied for the determination of the elements and one-factor-at-a-time method was employed for optimizing the ICP-MS parameters in migration experiment and microwave digestion experiment. The developed method was successfully applied to determine the content of 11 elements. The results showed that the experiment had excellent correlation and sensitivity. The accuracy of the elements in the migration study and test of soy sauce itself ranging from 84.25% to 118.75% was satisfied, and the precision of the method was validated and the RSD was no more than 15.5%. The concentration of all the detected metal elements migrated from the glass bottles were between 0.3450 and 2.398 ng·mL−1, and the risk assessment indicated that the metal elements in soy sauce had no risk to the public health. The proposed methodology in this study was successfully applied for the quality control for metal elements in soy sauce and the containing glass bottles for the first time, and a research method suitable for soy sauce consumption process control and risk assessment has been established.
{"title":"One-factor-at-a-time method combined with ICP-MS for determining 11 elements in soy sauce and their migration from the containing glass bottles","authors":"Xun Gao, Kexin Chen, Yue Zhang, Miaomiao Chi","doi":"10.1515/revac-2022-0031","DOIUrl":"https://doi.org/10.1515/revac-2022-0031","url":null,"abstract":"Abstract This study was designed to determine the 11 metal elements (Al, Cr, Mn, Fe, As, Ni, Cu, Zn, Cd, Sb, and Pb) in soy sauce and their migration from the containing glass bottles. Inductively coupled plasma mass spectrometry (ICP-MS) was applied for the determination of the elements and one-factor-at-a-time method was employed for optimizing the ICP-MS parameters in migration experiment and microwave digestion experiment. The developed method was successfully applied to determine the content of 11 elements. The results showed that the experiment had excellent correlation and sensitivity. The accuracy of the elements in the migration study and test of soy sauce itself ranging from 84.25% to 118.75% was satisfied, and the precision of the method was validated and the RSD was no more than 15.5%. The concentration of all the detected metal elements migrated from the glass bottles were between 0.3450 and 2.398 ng·mL−1, and the risk assessment indicated that the metal elements in soy sauce had no risk to the public health. The proposed methodology in this study was successfully applied for the quality control for metal elements in soy sauce and the containing glass bottles for the first time, and a research method suitable for soy sauce consumption process control and risk assessment has been established.","PeriodicalId":21090,"journal":{"name":"Reviews in Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":4.3,"publicationDate":"2021-12-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86724891","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
京公网安备 11010802042870号
京ICP备2023020795号-1
扫码关注我们
求助内容：
应助结果提醒方式：