超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查及定量分析保健品中11种非法添加降糖药物

Rapid screening and quantitative detection of 11 illegally added antidiabetics in health care products by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry

基于超高效液相色谱.四极杆／静电场轨道阱质谱建立了保健品中11种非法添加化学降糖药（那格列奈、盐酸吡格列酮、格列喹酮、格列齐特、格列吡嗪、格列本脲、盐酸二甲双胍、瑞格列奈、盐酸苯乙双胍、盐酸罗格列酮、格列美脲）的快速筛查和定量分析方法。样品采用甲醇提取，C18色谱柱（100 mm×4.6 mm，2.7μm）分离，用10 mmol／L乙酸铵水溶液和乙腈进行梯度洗脱，正离子模式扫描。化合物一级质谱的分辨率为70000，二级质谱分辨率为17500。实验结果表明，11种化合物在0.005～0.5 mg／L 范围内具有良好的线性（线性相关系数均大于0.99），各降糖类药物检出限为2.7～5.1μg／kg，回收率为87.3％～98.3％，相对标准偏差为2.18％～5.21％。本方法具有准确、简便、快速的特点，可用于降糖类保健品中11种降糖药物的定性筛查和定量分析。

A method for rapid screening and quantification of 11 antidiabetics （ nateglinide, pio.glitazone hydrochloride, gliquidone, gliclazide, glipizide, glibenclamide, metformin hydrochlo.ride, repaglinide, phenformin hydrochloride, rosiglitazone hydrochloride, glimepiride） illegally added in health care products by ultra performance liquid chromatography （ UPLC）.quadrupole/electrostatic field orbitrap mass spectrometry was established. The samples were extracted with methanol, and separated on an Agilent Poroshell 120 SB.C18 column （ 100 mm ×4.6 mm, 2.7μm） with acetonitrile.10 mmol/L ammonium acetate solution as mobile phases by gradient elu.tion. The positive mode was used in the MS detection. The resolution of the precursor mass was 70 000, while the resolution of the product mass was 17 500. The results indicated that the line.arity of all the 11 antidiabetics ranged from 0.005 mg/L to 0.5 mg/L with the correlation coeffi.cients greater than 0.99. The limits of detection were confirmed by spiked samples, and were between 2.7 and 5.1 μg/kg for the 11 antidiabetics. The recoveries were in the range of 87.3%to 98.3%, with the relative standard deviations in the range of 2.18%-5.21%. This method is accurate, simple and rapid, and can be used in rapid screening and quantitative analysis of the 11 illegally added antidiabetics in health care products.