超高效液相色谱-串联质谱法检测抗癫痫类中成药及保健食品中15种非法添加化学药物

目的 建立测定抗癫痫类中成药及保健食品中15种非法添加化学药物含量的超高效液相色谱-串联质谱(UHPLC-MS/MS)法.方法 供试品经甲醇提取,超声处理.色谱柱为ACES C18柱(150 mm×2.1 mm,1.7μm),流动相为10 mmol/L乙酸铵(0.1％甲酸)-乙腈(梯度洗脱),流速为0.3 mL/min...

Determination of 15 Chemical Drugs Illegally Added in Anti-Epilepsy Chinese Patent Medicines and Health Foods by UHPLC-MS/MS

Objective To establish an ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)method for the determination of 15 chemical drugs illegally added in anti-epilepsy Chinese patent medicines and health foods.Methods The samples were extracted with methanol by ultrasonic processing and separated on an ACES C18 column(150 mm×2.1 mm,1.7μm),the mobile phase was 0.1%formic acid in 10 mmol/L ammonium acetate-acetonitrile solution with gradient elution,and flow rate was 0.3 mL/min.The positive and negative ions were simultaneously scanned by electrospray ionization,and determined in the selective reaction monitoring mode.The chemical drugs were determined by comparing the molecular ion peaks,the second-order fragment ion peaks,the chromatographic retention time,and the content of the added drugs was calculated by the external standard method based on the peak area of the mass spectrum.Results The 15 kinds of illegally added chemical drugs were triazolam,midazolam,lorazepam,clonazepam,alprazolam,zaleplon,chlordiazepoxide,estazolam,oxazepam,diazepam,nitrazepam,secobarbital,phenobarbital,amobarbital and barbital,which showed good linearity in the range of 50-2000 ng/mL(r≥0.9991,n=7).The limit of detection(LOD)was in the range of 0.34-9.33 ng/g,the limit of quantitation(LOQ)was in the range of 1.13-31.11 ng/g,and the average recoveries were in the range of 96.77%-100.36%with RSDs of 1.07%-3.37%.The RSDs of precision,stability and repeatability tests were less than 4.00%.Among the sixteen batches of samples,diazepam illegally added in one batch was detected,and the content was 23.21 mg/g,phenobarbital illegally added in two batches was detected,and the contents were 15.35 mg/g and 17.89 mg/g,respectively.Conclusion The method is simple,accurate with high sensitivity,which can be used for rapid determination of illegally added chemical drugs in anti-epilepsy Chinese patent medicines and health foods.