HPLC-MS-MS法测定降糖类中成药中非法添加物格列波脲

Detection of glibornuride illegally added into traditional Chinese medicinal preparations by HPLC-MS-MS

目的建立液质联用法定性及定量测定降糖类中成药中非法添加格列波脲。方法液质联用定性筛查选用Dik-maSpursilC18柱（150mm×2．1mm，3μm），以甲醇-0．01mol/L乙酸铵溶液梯度洗脱，体积流量0．2mL／min。经液质联用筛查为阳性的样品用液相色谱进行定量测定，选用AgilentEclipsePlusC18柱（250mm×4．6mm，5μm），以甲醇-0．01mol／L乙酸铵溶液梯度洗脱，体积流量1mL／min，检测波长235nm。结果格列波脲在0．002～0．2mg／mL质量浓度范围内与峰面积有良好线性关系Y=217．88X＋0．3245，r2=0．9998，平均回收率为96．3％，RSD为1．0％（n=9）。结论通过对30多批次降糖类中成药进行测定，其中2批检测结果为阳性，含有量分别为5．8mg／g、3．5mg／g。

AIM To establish an HPLC-MS-MS method for qualitative and quantitative determining glibornuride illegally added into antidiabetic Chinese patent medicines. METHODS The qualitative analysis was performed on a Dikma Spursil Cls column （150 mm ×2. 1 mm, 3μm） of HPLC-MS/MS in gradient elution manner with the mobile phase of methanol -0. 01 mo]/L ammonium acetate, the flow rate of 0. 2 mlMmin. The positive sample detected by HPLC-MS/MS was determined with liquid chromatography , the test was conducted on Agilent Eclipse Plus C18 column （250 mm ×4.6 mm, 5 μm） in gradient elution manner with the mobile phase of methanol -0.01 moL/L ammonium acetate, the flow rate of lmL/min and the detection wavelengths was set at 235 nm. RE- SULTS The linear relationship was good in the range of 0. 002 - 0.2 mg/mL, and the linear equation was Y = 217.88X ＋0. 324 5, r2 =0. 999 8, the average recovery was 96.3% with the standard deviation of 1.0% （n = 9）. CONCLUSION The thirty batches of antidiabetic traditional Chinese medicinal preparations are determined. The results show that two batches present positive, and their contents are 5.8 mg/g and 3.5 mg/g, respec- tively.