消肿片中松香酸的HPLC和UPLC-MS/MS检测方法研究  

Detection of Abietic Acid in Xiaozhong Tablets by HPLC and UPLC-MS/MS

作　　者：刘益庆 钱明明 卢洋 杨颖 马秀建 Liu Yiqing;Qian Mingming;Lu Yang;Yangying;Ma Xiujian(Lianyungang Inspection Testing Center of Food and Drug,Jiangsu Lianyungang 222006,China)

机构地区：[1]连云港市食品药品检验检测中心,江苏连云港222006

出　　处：《中国药师》2020年第12期2502-2505,共4页China Pharmacist

基　　金：国家食品药品监督管理总局研究项目。

摘　　要：目的:建立消肿片中添加松香酸的HPLC和UPLC-MS/MS检测方法。方法:采用HPLC-DAD测定松香酸含量,色谱柱为SHISEIDO CAPCELL PAK C18(250 mm×4.6 mm,5μm);流动相为0.1%甲酸-乙腈-四氢呋喃(35:40:25),流速:1.0 ml·min-1;检测波长:241nm;柱温:25℃;进样量:10μl。采用UPLC-MS/MS方法对松香酸进一步确认,色谱柱为Agilent Poroshell120 EC-C18(2.1mm×50mm,2.7μm);流动相为0.1%甲酸-乙腈(30:70);进样量1μl;流速0.2ml·min-1。离子化模式为ESI+扫描,毛细管电压3500V,毛细管出口电压175V,干燥气温度:300℃,干燥气流速:8L·min-1,雾化器压力:35psig,碰撞能量15ev;扫描范围100~1 000m/z。结果:松香酸的线性范围为4.068~406.8μg·ml-1,r=0.999 9,平均回收率为100.88%,RSD为0.92%(n=9)。UPLC-MS/MS确认样品的一级质谱、二级质谱均与松香酸对照品一致。结论:该方法简便、准确、重复性好,适用于消肿片中非法添加松香酸的检查。Objective: To establish HPLC and UPLC-MS/MS methods to determine abietic acid added to Xiaozhong tablets.Methods: Using the column of Shiseido Capcell Pak C18( 250 mm×4.6 mm,5 μm) with 0.1% formic acid-acetonitrile-tetrahydrofuran( 35 ∶ 40 ∶ 25) as the mobile phase,the detection wavelength was 241 nm and the volume injection was 10 μl,the flow rate was 1.0 ml·min-1,and the column temperature was set at 30℃.To further confirm abietic acid,UPLC-Q-TOF-MS was performed on the column of Agilent Poroshell 120 EC-C18( 2.1 mm×50 mm,2.7 μm) with the mobile phase of 0.1% formic acid-acetonitrile( 30 ∶ 70) at a flow rate of 0.22 ml·min-1,and the volume injection was 1 μl. The ionization mode was ESI+,the capillary voltage was 3 500 V and the export voltage of capillary was 175 V. The drying gas temperature was 300℃ at the flow rate of 8 L·min-1,and the atomization gas pressure was 35 psig. The collision energy was 15 ev and the scan range was 100-1 000 m/z. Results: The linear range of Abietic acid was 4.068-406.8 μg·ml-1( r= 0.999 9),the average recovery was 100.88%,and the RSD was 0.92%( n= 9). UPLC-MS/MS confirmed that the primary and secondary mass spectra of samples were consistent with those of Abietic acid reference. Conclusion: The method is simple,accurate and reproducible,and suitable for the determination of Abietic acid in Xiaozhong tablets.

关 键 词：消肿片 松香酸 高效液相色谱-二极管阵列检测器 高效液相色谱-质谱联用 

分 类 号：R917[医药卫生—药物分析学]