Zheng Jia, Xi Cunxian, Cao Shurui, Wang Guomin, Tang Bobin, Wang Zhi, Mu Zhaode
College of Pharmacy, Chongqing Medical University, Chongqing 400016, China.
Chongqing Key Laboratory of Biochemistry and Molecular Pharmacology, Chongqing 400016, China.
Se Pu. 2017 Dec 8;35(12):1257-1265. doi: 10.3724/SP.J.1123.2017.09031.
A method for the simultaneous determination of 21 illegally added chemical drugs in improving sleep and immunity health foods using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. Oral liquid and health wine samples were shaken with acetonitrile and acetonitrile-water-formic acid (60:39:1, v/v/v), respectively, then purified by QuEChERS method. The extracts were separated on an Acquity UPLC BEH C18 column (50 mm×2.1 mm, 1.7 μm) with gradient elution of acetonitrile and 2 mmol/L ammonium acetate solution containing 0.1% (v/v) formic acid as mobile phases. The electrospray ionization in positive ion mode was used for analysis in multiple reaction monitoring (MRM) mode. The results showed that the target drugs had a good linear relationship in the range of 1-100 μg/L with the correlation coefficients () ≥ 0.992. The limits of detection (LODs) and limits of quantification (LOQs) were 0.07-3.41 μg/kg and 0.22-11.36 μg/kg, respectively. The average recoveries of the 21 chemical drugs in oral liquid and health wine were in the range of 61.4%-116.5% and 67.4%-98.4% with the relative standard deviations (RSDs) of 0.2%-13.4% and 0.2%-11.8%, respectively. The developed method is sensitive and reliable. It has been successfully used for the detection of illegally added chemical drugs in real samples.
建立了一种超高效液相色谱 - 串联质谱法（UPLC-MS/MS）同时测定改善睡眠和免疫类保健食品中21种非法添加化学药物的方法。口服液和保健酒样品分别用乙腈和乙腈 - 水 - 甲酸（60:39:1，v/v/v）振荡，然后采用QuEChERS方法进行净化。提取物在Acquity UPLC BEH C18柱（50 mm×2.1 mm，1.7 μm）上分离，以乙腈和含0.1%（v/v）甲酸的2 mmol/L醋酸铵溶液为流动相进行梯度洗脱。采用电喷雾电离正离子模式，在多反应监测（MRM）模式下进行分析。结果表明，目标药物在1 - 100 μg/L范围内具有良好的线性关系，相关系数（）≥0.992。检测限（LOD）和定量限（LOQ）分别为0.07 - 3.41 μg/kg和0.22 - 11.36 μg/kg。21种化学药物在口服液和保健酒中的平均回收率分别为61.4% - 116.5%和67.4% - 98.4%，相对标准偏差（RSD）分别为0.2% - 13.4%和0.2% - 11.8%。所建立的方法灵敏可靠，已成功用于实际样品中非法添加化学药物的检测。
