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Simultaneous Determination of 16 Illegally Added Drugs in Capsule Dietary Supplements Using a QuEChERS Method and HPLC–MS/MS
Chromatographia ( IF 1.7 ) Pub Date : 2021-09-07 , DOI: 10.1007/s10337-021-04087-y
Jinmei Gao 1 , Wenhui Gao 1 , Chunyan Ma 2 , Qiong Duan 2 , Hui Li 2
Affiliation  

A simple and rapid method based on the QuEChERS (quick, easy, cheap, effective, rugged, and safe) pretreatment and HPLC–MS/MS (high performance liquid chromatography–tandem mass spectrometry) system was successfully developed and validated for the analysis of 16 illegally added chemical drugs in capsule dietary supplements for weight-loss and lipid reduction. Samples were extracted with acetonitrile solution containing 1% formic acid. Then 500 mg mixed anhydrous magnesium sulfate and sodium chloride (1:1; m/m) were used for salting out, and 100 mg PSA adsorbents were used for purification. 16 analytes rendered good linearity in the range of 0.025–20 μg/g. The limits of detection (LOD) and limits of quantitation (LOQ) ranged from 0.3 to 20 ng/g and 1 to 50 ng/g, respectively. All the linear correlation coefficients were greater than 0.9942. The accuracy values of 16 analytes were between 80.21 and 118.35%, and the stability expressed by relative standard deviations (RSDs) were < 11.06% within three adding levels. Finally, fluoxetine was detected in 2 batch samples by the method. This method is simple, fast, practical and suitable for rapid detection of illegally added drugs in dietary supplements for weight loss and fat reduction. It also provides more powerful technical supports for the supervision of dietary supplements safety and can be used as an analytical method for the detection of such illegally added substances.



中文翻译:

使用 QuEChERS 方法和 HPLC-MS/MS 同时测定胶囊膳食补充剂中的 16 种非法添加药物

基于 QuEChERS(快速、简便、廉价、有效、耐用和安全)预处理和 HPLC-MS/MS(高效液相色谱-串联质谱)系统的简单快速方法被成功开发并验证用于分析减肥降脂胶囊膳食补充剂中非法添加化学药物16种。样品用含 1% 甲酸的乙腈溶液萃取。然后用500mg混合无水硫酸镁和氯化钠(1:1;m/m)盐析,用100mgPSA吸附剂提纯。16 种分析物在 0.025–20 μg/g 范围内呈现良好的线性。检测限 (LOD) 和定量限 (LOQ) 的范围分别为 0.3 至 20 ng/g 和 1 至 50 ng/g。所有线性相关系数均大于0.9942。16 种分析物的准确度值在 80.21 至 118.35% 之间,三个添加水平内的相对标准偏差 (RSD) 表示的稳定性< 11.06%。最后,通过该方法在2批样品中检测到氟西汀。该方法简单、快速、实用,适用于快速检测膳食补充剂中非法添加的减肥降脂药物。也为膳食补充剂的安全监管提供了更有力的技术支持,可作为检测此类非法添加物质的分析方法。快速、实用,适用于减肥减脂膳食补充剂中非法添加药物的快速检测。也为膳食补充剂的安全监管提供了更有力的技术支持,可作为检测此类非法添加物质的分析方法。快速、实用,适用于减肥减脂膳食补充剂中非法添加药物的快速检测。也为膳食补充剂的安全监管提供了更有力的技术支持,可作为检测此类非法添加物质的分析方法。

更新日期:2021-09-07
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