目的: 建立高效液相色谱-三重四级杆质谱(HPLC-MS/MS)法快速筛查及定量分析改善睡眠类保健品及中成药中22个精神类化合物。方法: 采用ZORBAX Eclipse Plus-C18 (2.1 mm×50 mm,1.8 μm)色谱柱进行分离,以乙腈-1 mmol·L-1乙酸铵(含0.1%甲酸)为流动相,梯度洗脱,流速为0.3 mL·min-1,电喷雾离子源,用多反应监测结合正离子扫描分析。通过比较样品与对照品的色谱保留时间、相对离子丰度比,进行定性分析,并对阳性样品进行定量分析。结果: 22个精神类化合物(阿普唑仑、地西泮、米安色林、帕罗西汀、氯丙嗪等)在0.1~400 ng·mL-1浓度范围呈良好的线性关系,线性相关系数大于0.99,样品回收率在79.1%~109.2%,RSD在1.2%~9.6%,检测下限范围在0.05~0.5 ng·mL-1。本方法可在13 min内同时完成对保健品和中成药中的22个精神类化合物的分离和筛查。检测12批次样品,结果均未检出22个精神类化合物。结论: 该方法操作简单,灵敏度高,准确可靠,可用于常见精神类化合物的快速检测。
Objective: To establish a rapid screening and quantitative analysis of 22 psychotropic compounds in health care products and Chinese patent medicines for improving sleep by high performance liquid chromatography-quadrupole mass spectrometry (HPLC-MS/MS). Methods: The supernatant was determined by LC-MS/MS using an ZORBAX Eclipse Plus-C18(2.1 mm×50 mm,1.8 μm) column with a gradient elution of 1 mmol·L-1 ammonium acetate (containing 0.1% formic acid) and acetonitrile. The flow rate was 0.3 mL·min-1. Electrospray ionization source was applied and operated in the multiple reaction monitoring mode. Qualitative analysis was carried out by comparing the chromatographic retention time and relative ion abundance ratio between the samples and the reference, and quantitative analysis was carried out on the positive samples. Results: The 22 psychotropic compounds (alprazolam, diazepam, mianserin, paroxetine, chlorpromazine, etc.) showed good linearity in the concentration range of 0.1-400 ng·mL-1, with the linear correlation coefficient greater than 0.99. The sample recoveries ranged from 79.1% to 109.2%, and RSD ranged from 1.2% to 9.6%. The lower limit of detection ranged from 0.05 to 0.5 ng·mL-1. The method can simultaneously separate and screen 22 mental compounds in health care products and Chinese patent medicines within 13 min. A total of 12 batches of samples were detected, without the detection of the 22 psychoactive compounds. Conclusion: The present method is simple, sensitive, accurate and reliable. It can be applied for screening the potential psychotropic compounds in medicines.
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