Chromatographic fingerprinting has been perceived as an essential tool for assessing quality and chemical equivalence of traditional Chinese medicine.However,this pattern-oriented approach still has some weak points i...Chromatographic fingerprinting has been perceived as an essential tool for assessing quality and chemical equivalence of traditional Chinese medicine.However,this pattern-oriented approach still has some weak points in terms of chemical coverage and robustness.In this work,we proposed a multiple reaction monitoring(MRM)-based fingerprinting method in which approximately 100 constituents were simultaneously detected for quality assessment.The derivative MRM approach was employed to rapidly design MRM transitions independent of chemical standards,based on which the large-scale fingerprinting method was efficiently established.This approach was exemplified on QiShenYiQi Pill(QSYQ),a traditional Chinese medicine-derived drug product,and its robustness was systematically evaluated by four indices:clustering analysis by principal component analysis,similarity analysis by the congruence coefficient,the number of separated peaks,and the peak area proportion of separated peaks.Compared with conventional ultraviolet-based fingerprints,the MRM fingerprints provided not only better discriminatory capacity for the tested normal/abnormal QSYQ samples,but also higher robustness under different chromatographic conditions(i.e.,flow rate,apparent pH,column temperature,and column).The result also showed for such large-scale fingerprints including a large number of peaks,the angle cosine measure after min-max normalization was more suitable for setting a decision criterion than the unnormalized algorithm.This proof-of-concept application gives evidence that combining MRM technique with proper similarity analysis metrices can provide a highly sensitive,robust and comprehensive analytical approach for quality assessment of traditional Chinese medicine.展开更多
Chinese herbal medicines（CHMs）are playing important roles in the treatment of diseases and human health care throughout the world.However,the extrinsic harmful residues have been threatening the therapies by destroy...Chinese herbal medicines（CHMs）are playing important roles in the treatment of diseases and human health care throughout the world.However,the extrinsic harmful residues have been threatening the therapies by destroying CHMs qualtiy which hinders the international trades of CHMs.This review summarized the extrinsic harmful residues contaminating CHMs in types,detection methods,national and international regulations,and made safety evaluations according to their contaminated levels,aiming to establish understanding among nations or organizations and provide references for the formulation or amendment of relative regulations.展开更多
建立了同时检测家禽肌肉组织中3种硝基咪唑类药物残留的液相色谱-串联质谱法。样品用乙酸乙酯提取,经浓缩、过滤后直接进入液相色谱-质谱分析。采用监测母离子及其相应子离子的多反应监测技术,根据离子流峰面积进行定量。3种药物的定量...建立了同时检测家禽肌肉组织中3种硝基咪唑类药物残留的液相色谱-串联质谱法。样品用乙酸乙酯提取,经浓缩、过滤后直接进入液相色谱-质谱分析。采用监测母离子及其相应子离子的多反应监测技术,根据离子流峰面积进行定量。3种药物的定量检出限分别为甲硝唑0.8μg/kg、洛硝哒唑0.1μg/kg、二甲硝唑0.1μg/kg。1次分析的运行时间为5 m in。是一种快速、灵敏、可靠的分析方法。展开更多
基金financially supported by the National Natural Science Foundation of China(Grant No.81803714)the Fundamental Research Funds for the Central Universities(Grant No.2019QNA7041).
文摘Chromatographic fingerprinting has been perceived as an essential tool for assessing quality and chemical equivalence of traditional Chinese medicine.However,this pattern-oriented approach still has some weak points in terms of chemical coverage and robustness.In this work,we proposed a multiple reaction monitoring(MRM)-based fingerprinting method in which approximately 100 constituents were simultaneously detected for quality assessment.The derivative MRM approach was employed to rapidly design MRM transitions independent of chemical standards,based on which the large-scale fingerprinting method was efficiently established.This approach was exemplified on QiShenYiQi Pill(QSYQ),a traditional Chinese medicine-derived drug product,and its robustness was systematically evaluated by four indices:clustering analysis by principal component analysis,similarity analysis by the congruence coefficient,the number of separated peaks,and the peak area proportion of separated peaks.Compared with conventional ultraviolet-based fingerprints,the MRM fingerprints provided not only better discriminatory capacity for the tested normal/abnormal QSYQ samples,but also higher robustness under different chromatographic conditions(i.e.,flow rate,apparent pH,column temperature,and column).The result also showed for such large-scale fingerprints including a large number of peaks,the angle cosine measure after min-max normalization was more suitable for setting a decision criterion than the unnormalized algorithm.This proof-of-concept application gives evidence that combining MRM technique with proper similarity analysis metrices can provide a highly sensitive,robust and comprehensive analytical approach for quality assessment of traditional Chinese medicine.
基金supported by CAMS Innovation Fund for Medical Sciences (No. 2016-I2M-1-012, 2017-I2M-1-013)National Natural Science Foundation of China (No. 81573595, 81703699)National Project for Standardization of Chinese Materia Medica (No. ZYBZH-Y-JIN-34)
文摘Chinese herbal medicines（CHMs）are playing important roles in the treatment of diseases and human health care throughout the world.However,the extrinsic harmful residues have been threatening the therapies by destroying CHMs qualtiy which hinders the international trades of CHMs.This review summarized the extrinsic harmful residues contaminating CHMs in types,detection methods,national and international regulations,and made safety evaluations according to their contaminated levels,aiming to establish understanding among nations or organizations and provide references for the formulation or amendment of relative regulations.
文摘建立了同时检测家禽肌肉组织中3种硝基咪唑类药物残留的液相色谱-串联质谱法。样品用乙酸乙酯提取,经浓缩、过滤后直接进入液相色谱-质谱分析。采用监测母离子及其相应子离子的多反应监测技术,根据离子流峰面积进行定量。3种药物的定量检出限分别为甲硝唑0.8μg/kg、洛硝哒唑0.1μg/kg、二甲硝唑0.1μg/kg。1次分析的运行时间为5 m in。是一种快速、灵敏、可靠的分析方法。
