HPLC-MS-MS法测定降糖类中成药中非法添加物格列波脲-申国华-董培智-裴社.pdf

网络出版时间：2013-12-09 15:48 网络出版地址：/kcms/detail/31.1368.R1548.001.html HPLC-MS-MS 法测定降糖类中成药中非法添加物格列波脲 1 申国华，董培智，裴社强，郭景文，行江水 （山西省食品药品检验所，山西 太原 030001） 摘要：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Dikma Spursil C18 柱(150 mm×2.1 mm,3 μ m)，以甲醇-0.01 mol/L 乙酸铵溶液梯度洗脱,体积流量0.2 mL/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 Agilent Eclipse Plus C 柱（250 mm×4.6 mm，5 μ m），以甲醇-0.01mol/L 乙酸铵溶液梯度洗脱, 18 体积流量 1mL/min ，检测波长 235 nm 。结果 格列波脲在 0.002～0.2 mg/mL 质量浓度范围内与峰面积有良好线性关系 2 Y=217.88X+0.3245，r =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5.8 mg/g、3.5 mg/g。 关键词：液质联用；中成药；非法添加；格列波脲： Detection of Glibornuride illegally added into traditional Chinese medicinal preparations by HPLC-MS-MS SHEN Guo-hua, DONG Pei-zhi, PEI She-qiang, GUO Jing-wen, XING Jiang-shui (Shanxi Provincial Institute for Food and Drug Control, Taiyuan 030001 ,china ) ABSTRACT: AIM An HPLC-MS-MS method of qualitative and quantitative method for determing the illegally added Glibornuride into antidiabetic Chinese patent medicine. METHODS The qualitative analysis was performed on a Dikma Spursil C18 column (150 mm×2.1 mm,3 μm) of HPLC-MS/MS in gradient elution manner with the mobile phase of methanol -0.01 mol/L ammonium acetate ，the flow rate of 0.2 mL/min. The positive sample detected by HPLC-MS/MS was determined with liquid chromatography ,the test was conducted on Eclipse Plus C18 column (250 mm×4.6 mm,5 μm) in gradient elution wanner with the mobile phase of methanol -0.01 mol/L ammonium acetate, the flow rate of 1mL/mi