摘要:
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,1.9 μm)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。
Abstract:
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, 1.9 μm) 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.
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