液相色谱-串联四极杆质谱测定中药及保健品中非法添加8种化学降糖药

Detection of 8 kinds of Antidiabetics Illegally Added in Traditional Chinese Medicinal Preparations and Health Foods by the Liquid Chromatography Tandem with Quadrupole Mass Spectrometry Method

目的建立液相色谱-串联四极杆质谱法检测降糖类中药及保健食品违禁添加的8种化学药物。方法采用ZORBAX SB-C18柱,分别以0.1%甲酸（用氨水调节pH至3.5）-乙腈进行梯度洗脱,检测波长240nm,采用正离子扫描模式,8种药物的检测限为0.5~8ng.mL-1,通过与标准图库中保留时间和MRM图谱比较,以及参照一级、二级图谱比较,筛查出样品中违法违禁添加的8种药物,并通过MRM模式,对供试品进行初步定量。结果与结论在103批供试品中,分别检测到二甲双胍、苯乙双胍、格列本脲、盐酸格列吡嗪、格列齐特、格列喹酮等8种化学降糖药。

Objective To develop a method for the identification of 8 kinds of antidiabetics illegally added in traditional Chinese medicine and health foods.Methods ZORBAX SB-C18 column was used,together with the mobile phase of 0.1% formic acid（adjusted to pH 3.5 with ammonium hydroxide） and acetonitrile by gradient elution.The detection wavelength was 240nm;positive scan.The LOD（limit of detection） is 0.5～8ng·mL-1.Compared with the retention time of standard MRM chromatograph,and the MS1 and MS2 spectrum of reference standard,we determined and quantitated 8 kinds of antidiabetics under MRM methods.Results Conclusion In the 103 batches of samples,8 kinds of antidiabetics were detected.