摘要
目的建立用于改善睡眠类保健食品中非法添加卡马西平、氯丙嗪、舒必利、奥卡西平、奥氮平、多赛平和喹硫平7种化学药品的HPLC快速筛查方法。方法采用HPLC法,C18柱进行分离(250 mm×4.6 mm;5μm);检测波长:250 nm;柱温:35℃。流动相:甲醇-0.02 mol/L磷酸二氢钾溶液,梯度洗脱。结果经对建立的HPLC法进行方法学考察,7种目标分析物的线性范围为20-600μg/ml,检出限为0.4-2.5 ng/g,定量限为2.5-5.0 ng/g;方法的重复性(RSD)在0.1%-3.6%之间,仪器精密度(RSD)在0.2%-2.8%之间;平均回收率为95-102%;7个成分的溶液在32 h内基本稳定。结论该HPLC法操作简便,能同时快速筛查保健食品中卡马西平等7种非法添加化学药品。
Objective To establish a rapid screening method for the simultaneous determination of 7 kinds of illegally-added chemical drugs,including Carbamazepine,Chlorpromazine,Sulpiride,Oxcarbazepine,Olanzapine,Doxepin and Quetiapine,in improving sleep quality health food by high performance liquid chromatography( HPLC). Methods A C18 column( 250 mm × 4. 6 mm,5 μm)was used for chromatographic separation,which was eluted with methanol-0. 02 mol/L potassium dihydrogen phosphate as mobile phase at 35 ℃. The diode array detector was used for detection at 250 nm. Results The 7 chemical drugs showed a linear relationship in the range of 20-600 μg/ml. The limit of determination and the limit of quantification of the method were in the ranges of 0. 4-2. 5 ng/g and 2. 5-5. 0 ng/g,respectively. The RSD of repeatability was in the range of 0. 1%-3. 6% and the precision of instrument was 0. 2%-2. 8%. The average recovery rate was 95%-102%. The above seven components solution was stable in 32 h.Conclusion This method is simple and convenient,and suitable for simultaneous rapid determination of 7 kinds of illegally-added chemical drugs in health food.
出处
《山西医科大学学报》
CAS
2017年第11期1165-1168,共4页
Journal of Shanxi Medical University
关键词
改善睡眠类保健食品
HPLC
非法添加化学药品
improving sleep quality health food
high performance liquid chromatography
illegally-added chemical drugs