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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 |
| 阅读数： | 633 次 |
| 本月下载数： | 4 次 |
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