高效液相色谱检查中药及保健品中添加苯巴比妥等8种镇静催眠药的研究  

Detection of Phenobarbital and Seven Other Sedative Hypnotics Illegally Adulterated into Traditional Chinese Medicines and Health Foods by HPLC-DAD

作　　者：金鹏飞[1] 王志宏[1] 王伟夫[2] 邹定[1] 马捷[1] 胡欣[1] 

机构地区：[1]卫生部北京医院药学部,北京100730 [2]总参谋部警卫局卫生保健处,北京100017

出　　处：《中国药学杂志》2012年第6期462-466,共5页Chinese Pharmaceutical Journal

基　　金：中央保健科研课题专项资金(B2009B032)

摘　　要：目的应用高效液相色谱-二极管阵列检测器(HPLC-DAD),建立中药及保健品中添加的苯巴比妥、咪达唑仑、艾司唑仑、奥沙西泮、硝西泮、阿普唑仑、氯硝西泮和地西泮的检查方法。方法采用Alltima C18色谱柱(4.6 mm×250 mm,5μm),以10 mmol.L-1磷酸二氢铵溶液(磷酸调至pH 2.7)-乙腈(65∶35)或10 mmol.L-1磷酸二氢铵溶液(磷酸调至pH 2.7)-甲醇(40∶60)为流动相,流速0.5 mL.min-1,检测波长220 nm。结果苯巴比妥、咪达唑仑、艾司唑仑、奥沙西泮、硝西泮、阿普唑仑、氯硝西泮和地西泮在5～320 mg.L-1内线性关系良好,线性相关系数(r)都大于0.999 7;灵敏度高,最低检测限都在4.3～13.0 ng.mL-1之间;回收率良好,低、中、高3个浓度的回收率都在98.08%～102.1%之间;精密度良好,相对标准偏差(RSD)均小于1.58%;稳定性良好,12 h内峰面积和保留时间的相对标准偏差(RSD)均小于1.05%和0.54%。对19种不同剂型样品的检测结果显示:在两种保健品胶囊中检出硝西泮。结论该方法快速、灵敏、易推广,可作为中药及保健品中非法添加8种镇静催眠药的检查方法。OBJECTIVE To establish an HPLC-DAD method for the detection of midazolam, phenobarbital, estazolam, oxaze- pam, nitrazepam, alprazolam, clonazepam and diazepam illegally adulterated into traditional Chinese medicines and health foods. METHODS An Alltima CI8 column （4. 6 mm x250 ram,5 Ixm） was used for the separation with 10 mmol ~ L-I ammonium dihydro- gen phosphate （ adjusted pH to 2. 7 with H3 PO4 ） - aeetonitrile （65：35 ） or 10 mmo] ~ L -~ ammonium dibydrogen phosphate （ adjusted pH to 2. 7 with H3P04） - methanol （40： 60） as the mobile phase at the flow rate of 0. 5 mL ~ rain-~. The detection wavelength was 220 nm. RESULTS The method showed good linearity and sensitivity for the 8 compounds with all correlation coefficients （r） greater than 0. 999 7 and all LODs between 4. 3 - 13.0 ng mL-t ; the spiked recoveries of low, middle and high levels ranged from 98. 08% to 102. 1% ; the precisions were satisfactory with all RSDs lower than 1.58% ; the stability within 12 h was acceptable with the RSDs of peak areas and retention times no more than 1.05% and 0. 54%. In the test of 19 samples of different dosage forms, nitrazepam was found in two health foods. CONCLUSION This method is fast, sensitive and propagable for the detection of 8 sedative hypnotics il- legally adulterated into traditional Chinese medicines and health foods.

关 键 词：高效液相色谱-二极管阵列检测器 中药 保健品 镇静催眠药 苯巴比妥 苯二氮 咪达唑仑 艾司唑仑 

分 类 号：R917[医药卫生—药物分析学]