降压类中成药及保健食品中21种非法添加化学药物的快速检测与确证方法研究

Rapid Detection and Conformation of 21 Illegal Chemical Drugs in Antihyertension Traditional Chinese Medicine and Healthy Food

采用亚3μm色谱柱建立了降压类中成药及保健食品中21种非法添加化学药物的高效液相色谱快速检测及液相色谱-质谱联用确证方法。样品经甲醇-乙腈（体积比5∶5）超声提取,采用Agilent Poroshell 120Phenyl-Hexyl（100 mm×4.6 mm,2.7μm）色谱柱,以甲醇-乙腈（体积比2∶1）-甲酸水溶液（pH 2.5±0.1）为流动相,梯度洗脱,二极管阵列检测器检测,外标法定量,液质联用法进一步定性确证。结果表明,21种成分在17 min内完成分离,方法检出限为0.03～0.50 mg/g,定量下限为0.09～1.50 mg/g,平均回收率为82.0%～109.0%。采用上述方法对107批从互联网收集的样品进行检测,阳性检出率为42.1%。该方法快速、准确,适用于降压类中成药及保健食品中非法添加药物的快速检测。

A method was developed for the determination and conformalion of 21 illegal chemical drugs in antihypertension traditional Chinese medicines and health care foods by HPLC - DAD and LC -MS/MS with sub -3 μm particle colmnn. The samples were extracted with methanol -acetonitrile （5 ： 5, by volume）, then separated on an Agilent Poroshell 120 phenyl- Hexyl（ 100 mm ×4.6 mm, 2.7 μm） by gradient elution with methanol -acetonitrile（2 ：1 , by volume） - formic acid wa- ter solution（pH 2.5 ± 0. 1 ） as mobile phase, detected with DAD in wavelength range of 200 - 400 nm. Quantification analysis were performed by the external standard method. The positive samples were further identified and verified by LC - MS/MS. The results indicated that 21 analytes were sepa- rated completely in 17 min. The detection limits of 21 target compounds ranged from 0.03 mg/g to 0. 50 mg/g. The average recoveries at three spiked levels ranged from 82.0% to 109.0%. The method was applied in the analysis of 107 batches of samples from online shopping, among which 45 batches were added with the chemicals with a positive rate of 42. 1%. The method was accurate, rapid and sensitive, and was suitable for the determination of illegally added chemical drugs in tradi- tional Chinese medicine and healthy food of antihypertension.