高效液相色谱-串联质谱法快速测定降压类中成药及保健食品中非法添加12种化学药物的研究

Rapid detection of 12 kinds of chemical drugs illegally added in antihypertensive traditional Chinese medicines and health care foods by high performance liquid chromatography tandem mass spectrometry

目的建立一种快速、准确的高效液相色谱-串联质谱技术(LC-MS/MS)同时测定中成药与保健食品中非法添加的12种降压类化学药物。方法样品经甲醇提取,超声处理后,采用LC-MS/MS法,以Agilent Eclipseplus C18(50 mm×2.1 mm,1.8μm)为色谱柱,0.1%甲酸甲醇溶液(A)-0.1%甲酸水溶液(B)为流动相,采用ESI正离子源并在多反应监测(MRM)模式下测定,通过比较分子离子峰、二级碎片离子峰、色谱保留时间等信息确定添加的化学药物,并根据外标法以质谱峰面积计算添加药物的准确量。结果12种化学药物阿替洛尔、可乐定、氢氯噻嗪、卡托普利、哌唑嗪、利血平、硝苯地平、氨氯地平、尼群地平、尼莫地平、尼索地平、非洛地平分离度良好,在1 ng/ml^500 ng/ml质量浓度内具有良好的线性关系(r≥0.9980),方法检出限(LOD)为0.005 ng/g^0.52 ng/g,定量限(LOQ)为0.021 ng/g^1.63 ng/g,回收率为83.2%~117.3%,相对标准偏差为0.8%~6.7%。结论本法简便、准确、灵敏度高,可作为降压类中成药及调节血压类保健食品中非法添加化学降压药的快速检验方法。

Objective A fast and accurate method was developed for the determination and conformation of 12 kinds of chemical drugs illegally added in antihypertension traditional Chinese medicines and health care foods by LC-MS/MS.Methods The samples were extracted with methanol by ultrasonic processing and separated on a Agilent Eclipseplus C18(50 mm×2.1 mm,1.8μm)column with methanol(A)and 0.1%formic acid water solution.The chemical hypotensors were determined by LC-MS-MS in positive ionization and multiple reaction monitoring mode.The obtained molecularions,fragment ions,and retention time for MRM channels were used to identify the 12 kinds of drugs,and quantitative analysis was conducted with external standard method.Results This method had a good separation effect,the 12 kinds of chemical drugs,including atenolol,Clonidine,hydrochlorothiazide,captopril,prazosin,reserpine,nifedipine,amlodipine,nitrendipine,nimodipine,nisoldipine,felodipine showed good linearity with the correlation coefficients≥0.9980.The limits of detection and quantitative were in the range of 0.005 ng/g-0.52 ng/g and 0.021 ng/g-1.63 ng/g.The recoveries were within 83.2%-117.3%,and the relative standard deviations were within 0.8%-6.7%.Conclusion This method is simple,accurate with high sensitivity,which was suitable for rapid determination of the 12 kinds of chemical drugs which illegally added in antihypertension traditional Chinese drugs and blood pressure regulation health foods.