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
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篇名: 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
TITLE:
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5 μl。质谱条件:离子源为电喷雾电离源,毛细管电压为4.0 kV,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2.0~32 μg/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3.0~48 μg/L,其余14种化学物质检测质量浓度线性范围为2.5~40 μg/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。
ABSTRACT: OBJECTIVE: To establish a method for the detection of 24 chemical substances that illegally added into antihypertensive 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, column 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, desolvation 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 2.0-32 μg/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). CONCLUSIONS: The method is specific, sensitive, simple and rapid, and suitable for the detection of chemical substances that illegally added into antihypertensive traditional Chinese medicines.
期刊: 2016年第27卷第33期
作者: 凌海燕,汤燕,朱宁,杨军,文筱,杨安东
AUTHORS: LING Haiyan,TANG Yan,ZHU Ning,YANG Jun,WEN Xiao,YANG Andong
关键字: 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
KEYWORDS: HPLC-Q-TOF-MS/MS; Antihypertensive traditional Chinese patent medicine; Chemical substances; Illegal added
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