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投稿时间:2018-10-22
投稿时间:2018-10-22
中文摘要: 建立同时检测保健食品中非法添加的13 种化学降糖药物的液相色谱串联质谱分析方法并用于实际检测。保健食品样品经甲醇超声提取后,以色谱柱(2.1 mm×150 mm,5 μm)进行分离,甲醇和10 mmol/L 乙酸铵水溶液(含0.1%甲酸)为流动相梯度洗脱;采用电喷雾电离源正离子(electrospray ionization positive,ESI+),多反应监测(multiple reaction monitoring,MRM)模式进行检测。13 种化学降糖药物线性相关系数均大于0.999,定量限(limits of quantitation,LOQ)为45.7 μg/kg~79.6 μg/kg,回收率为 78.6%~112.1%,相对标准偏差(relative standard deviations,RSD)为 0.6%~3.5%。从11 种样品中检测出5 种样品含非法添加化学药物,且均为复合添加。2 种样品添加二甲双胍,5 种样品添加苯乙双胍,2 种样品添加罗格列酮,1 种样品添加甲苯磺丁脲,1 种样品添加吡格列酮,5 种样品添加格列本脲。
中文关键词: 高效液相色谱-串联质谱 降糖类保健食品 化学降糖药 辅助降血糖 含量测定
Abstract:To develop and apply a method for the simultaneous determination of 13 kinds of illegal drugs in antidiabetic supplements by using high performance liquid chromatography-tandem mass spectrometry(HPLCMS/MS).The samples were extracted using methanol.The target analytes were separated on column(2.1 mm×150 mm,5 μm)with a mobile phase consisting of 10 mmol/L ammonium acetate(including 0.1%formic acid)and methanol by gradient elution.The detection was determined based on ESI+(electrospray ionization positive)and MRM (multiple reaction monitoring) mode.The results showed good linear relationships with the correlation coefficients larger than 0.999 for all 13 kinds of illegal drugs.The limits of quantitation (LOQ)were all in the range of 45.7 μg/kg-79.6 μg/kg.The recoveries were in the range of 78.6 %-112.1 % with relative standard deviations (RSD)of 0.6 %-3.5 % at three spiked levels.In the 11 batches of samples,the illegal synthetic drugs were found in 5 samples and all the 5 samples contain more than one illegal synthetic drug;in which metformin was found in two samples,phenformin was found in five samples,rosiglitazone was found in two samples,tolbutamide was found in one sample,pioglitazone was found in one sample,glidenclamide was found in five samples.
keywords: high performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS) antidiabetics supplements antidiabetics drugs auxiliary hypoglycemic determination
文章编号:201919035 中图分类号: 文献标志码:
基金项目:湖北省食品药品监督管理局科研项目(201602011)
Author Name | Affiliation |
QIN Juan,XIE Bai-yan,YANG Yu-ping,WANG Lin,LEI Ji-yuan,PENG Shu-xiang,TU Lin* | Wuhan Institute for Drug and Medical Device Control,Wuhan 430075,Hubei,China |
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