HPLC-Q-TOF-MS/MS法检测降压类中成药中非法添加的24种化学物质  

Detecion of 24 Chemical Substances that Illegally Added into Antihypertensive Traditional Chinese Patent Medicines by HPLC-Q-TOF-MS/MS

作　　者：凌海燕[1] 汤燕[1] 朱宁[1] 杨军[1] 文筱[1] 杨安东[1] 

机构地区：[1]四川省中医药科学院,成都610041

出　　处：《中国药房》2016年第33期4712-4715,共4页China Pharmacy

基　　金：四川省公益性科研院所基本科研项目(No.A-2015N-7)

摘　　要：目的：建立检测降压类中成药中非法添加的24种化学物质的方法。方法：采用高效液相色谱-飞行时间串联质谱法。色谱条件：色谱柱为Agilent Poroshell 120 EC-C18,流动相为0.05%甲酸溶液-甲醇（梯度洗脱）,流速为0.3 ml/min,柱温为30℃,进样量为5μl。质谱条件：离子源为电喷雾电离源,毛细管电压为4.0 k V,毛细管出口电压为135 V,锥孔电压为65 V,脱溶剂温度为350℃,干燥气流速为10 L/min,雾化器压力为40 psi,碰撞能量为8-45 V,扫描范围为m/z 100-1 700,检测方式为正离子模式（ESI＋）。结果：卡托普利、硝苯地平、氢氯噻嗪、盐酸可乐定、利血平检测质量浓度线性范围为2.0-32μg/L,苯磺酸氨氯地平、非洛地平、缬沙坦、拉西地平、坎地沙坦酯检测质量浓度线性范围为3.0-48μg/L,其余14种化学物质检测质量浓度线性范围为2.5-40μg/L（r≥0.995 9）;定量限≤2.944 1 ng,检测限≤0.988 5 ng;精密度、稳定性、重复性试验的RSD≤5.1%;回收率为81.5%-115.5%（RSD=1.81%-4.86%,n=9）。结论：该方法专属性强、灵敏度高、简便快捷,适用于降压类中成药中非法添加化学物质的检测。OBJECTIVE： To establish a method for the detection of 24 chemical substances that illegally added into antihyper- tensive traditional Chinese medicines. METHODS： HPLC-Q-TOF-MS/MS was adopted. The chromatographic conditions were as follows, the column was Agilent Poroshell 120 EC-C18 with mobile phase of 0.05% formic acid-methanol （gradient elution） at a flow rate of 0.3 ml/min, colunm temperature was 30 ℃, injection volume was 5 μl. MS conditions were as follows, ion sou- rce was an electrospray ionization source, capillary voltage was 4.0 kV, capillary exit voltage was 135 V, cone voltage was 65 V, de- solvation temperature was 350 ℃, drying gas flow rate was 10 L/min, nebulizer pressure was 40 psi, collision energy was 8-45 V; scanning range was m/z 100-1 700; and detection method was positive ion mode （ESI＋）. RESULTS： The linear range was 2.0-32μg/L for captopril nifedipine, hydrochlorothiazide, clonidine hydrochloride, reserpine, 3.0-48 μg/L for amlodipine besylate, felodipine,valsartan, lacidipine, candesartan cilexetil and 2.5-40 μg/L for the other 14 chemical substances （r≥0.995 9）; limit of quantification was not higher than 2.944 1 ng,the limit of detection was not higher than 0.988 5 ng; RSDs of precision, stability and reproducibility tests were no higher than 5.1%; recoveries were 81.5%-115.5% （RSD were 1.81%-4.86%, n=9）. CONCLU- SIONS： The method is specific, sensitive, simple and rapid, and suitable for the detection of chemical substances that illegally add- ed into antihypertensive traditional Chinese medicines.

关 键 词：高效液相色谱-飞行时间串联质谱法 降压类中成药 化学物质 非法添加 

分 类 号：R917[医药卫生—药物分析学]