摘要
建立了生化药品、中成药和保健品中非法添加的13种消化类化学药的超高效液相色谱-Orbitrap高分辨质谱(UHPLC-HRMS)高通量筛查方法。供试品以甲醇-水(50∶50)为提取溶剂,经Hypersil Gold C18(2.1 mm×100 mm,3μm)色谱柱分离,以乙腈-0.1%甲酸水为流动相进行梯度洗脱,单次分析仅需10min。采用正离子检测,Full MS/dd-MS2扫描模式。通过比较供试品与对照品的色谱保留时间、高分辨一级和二级质谱,判断供试品中是否非法添加消化类药物,并对阳性样品进行定量分析。13种化合物的线性范围均为8.0~800μg/L,相关系数(r)均不低于0.998 5,回收率为94.6%~106.2%,相对标准偏差为1.2%~2.9%。该法快速简便、通量高、选择性好、灵敏度高,并已用于生化药品、中成药及保健品非法添加消化类化学药的高通量筛查和测定,在38批中成药中发现5批阳性样品,在43批保健品中发现3批阳性样品。
A method was established for the high-throughput screening of 13 digestive drugs adulterated in biochemical drugs,Chinese patent medicines and dietary supplements by high-performance liquid chromatography-Orbitrap high resolution mass spectrometry(UHPLC-HRMS).Samples were extracted with methanol-water(50∶50,by volume),chromatographically separated on a Hypersil Gold C 18(2.1 mm×100 mm,3μm)column with acetonitrile-0.1%formic acid as mobile phase by gradient elution.The analysis time for a single injection was merely 10 min.MS detection was performed in positive ion Full MS/dd-MS 2 scan mode.Comparing the chromatographic retention time,high resolution primary and secondary mass spectra of the sample with those of the reference substance,it could be judged whether the digestive drug was adulterated into the test samples or not,and the positive samples were quantified.The linear ranges for these 13 digestive drugs were all 8.0-800μg/L with their correlation coefficients(r)no less than 0.998 5.The recoveries were over the range of 94.6%-106.2%with relative standard deviations of 1.2%-2.9%.With the advantages of rapidness,simplicity,high-throughput,good selectivity and high sensitivity,this method was used for the high-throughput screening and determination on 13 kinds of digestive chemicals adulterated in biochemical drugs,Chinese patent medicines and dietary supplements.Five batches of positive samples were found in 38 batches of Chinese patent medicines,and three batches of positive samples were found in 43 batches of dietary supplements.
作者
郭常川
孙华
石峰
邢晟
张迅杰
李可
贺美莲
姜玮
GUO Chang-chuan;SUN Hua;SHI Feng;XING Sheng;ZHANG Xun-jie;LI Ke;HE Mei-lian;JIANG Wei(Shandong Institute for Food and Drug Control,Jinan 250101,China;College of Pharmaceutical Sciences, Shandong University,Jinan 250012,China;School of Chemistry and Chemical Engineering,Shandong University,Jinan 250100,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2018年第3期300-306,共7页
Journal of Instrumental Analysis
关键词
消化药
非法添加
Orbitrap高分辨质谱
测定
高通量筛查
digestive drug
illegally adulteration
Orbitrap high resolution mass spectrometry
determination
high-throughput screening
