摘要
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ACESC_(18)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;电喷雾电离正、负离子同时扫描,并在选择反应监测模式下测定,通过比较分子离子峰、二级碎片离子峰、色谱保留时间等确定添加的化学药物;并根据外标法以质谱峰面积计算添加药物的含量。结果15种非法添加化学药物分别为三唑仑、咪达唑仑、劳拉西泮、氯硝西泮、阿普唑仑、扎来普隆、氯氮卓、艾司唑仑、奥沙西泮、地西泮、硝西泮、司可巴比妥、苯巴比妥、异戊巴比妥、巴比妥,质量浓度均在50~2000 ng/mL范围内与峰面积线性关系良好(r≥0.9991,n=7);检测限为0.34~9.33 ng/g,定量限为1.13~31.11 ng/g;平均加样回收率为96.77%~100.36%,RSD为1.07%~3.37%;精密度、稳定性、重复性试验的RSD均小于4.00%。16批样品中,1批检出非法添加地西泮,含量为23.21 mg/g;2批检出非法添加苯巴比妥,含量分别为15.35 mg/g,17.89 mg/g。结论该方法操作简便,结果准确,灵敏度高,可用于快速检测抗癫痫类中成药及保健食品中非法添加的化学药物。
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.
作者
王超众
南俊伶
王萌萌
刘信奎
刘春峰
于百青
初红涛
WANG Chaozhong;NAN Junling;WANG Mengmeng;LIU Xinkui;LIU Chunfeng;YU Baiqing;CHU Hongtao(Heilongjiang University of Chinese Medicine,Harbin,Heilongjiang,China 150040;Qiqihar Institute for Drug Control,Qiqihar,Heilongjiang,China 161005;The First Hospital of Qiqihar,Qiqihar,Heilongjiang,China 161005;Qiqihar University,Qiqihar,Heilongjiang,China 161006)
出处
《中国药业》
CAS
2022年第1期55-59,共5页
China Pharmaceuticals
基金
黑龙江省自然科学基金[YQ2019H034]
黑龙江省中医药科研项目[ZHY2020-009]
黑龙江省齐齐哈尔市科技计划创新激励项目[CSFGG-2020220]。
