超高效液相色谱串联质谱法同时测定减肥类保健食品中10种非法添加利尿类及泻下类药物

Simultaneous Determination of 10 Diuretics and Laxatives Illegally Added in Slimming Health Foods by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

建立一种减肥类保健食品中10种非法添加利尿类及泻下类药物的超高效液相-串联质谱(UPLC-MS/MS)测定方法。样品用甲醇超声提取,再经甲醇10倍稀释后,采用Thermo Hypersil GOLD色谱柱(100 mm×2.1 mm,1.9μm)分离,以水-乙腈为流动相进行梯度洗脱,多反应监测10种非法添加药物(氯噻嗪、氢氯噻嗪、氯噻酮、甲氯噻嗪、吲达帕胺、酚酞、芦荟大黄素、比沙可啶、大黄酚、大黄素)。结果显示10种非法添加药物在0.92~148.8 ng/mL范围内线性关系良好,相关系数(R2)均大于0.995,平均回收率70%~125%。所检13批样品中3批检出非法添加酚酞、2批检出非法添加氢氯噻嗪,阳性率为38%。本方法准确,灵敏度高,专属性好,检出限低,可用于减肥类保健食品中10种非法添加药物的定性及定量测定。

A method for simultaneous determination of 10 diuretics and laxatives illegally added in slimming health foods by UPLC-MS/MS was developed.The sample was extracted by methol with ultrasound extraction.After diluted 10 times by methol,the sample was separated on thermo hypersil GOLD(100 mm×2.1 mm,1.9μm)column with the gradient elution.The mobile phase consisted of water and acetonitrile.Multiple reactions monitoring mode was used to quantify the 10 illegally added drugs(chlorothiazide,hydrochlorothiazide,piperacillin,methyclothiazide,indapamide,phenolphthalein,aloe-emodin,bisacodyl,emodin,chrysophanic acid).10 kinds of illegal drugs had good linear relationship in the range of 0.92~148.8 ng/mL,the correlation coefficients(R2)were greater than 0.995,and the average recoveries were 70%~125%.Furosemide was detected in 3 batches and hydrochlorothiazidel was detected in 2 batch of 13 samples.The positive rate was 38%.This method is accurate,sensitive,specific,and low detection limit.It can be used for the qualitative and quantitative determination of 10 drugs illegally added in slimming health foods.