安神类保健食品中新型非法添加药物的检测研究
目的 建立超高效液相色谱法(UPLC)及气相色谱-质谱(GC-MS)法, 用于检测并确证安神类保健食品中的新型非法添加药物。方法 采用溶剂超声或液-液萃取方式对样品进行提取后, 采用UPLC进行测定。UPLC采用ZORBAX SB-C18(2.1×150 mm, 1.8 μm)色谱柱分离, 采用乙腈和0.1%磷酸溶液为流动相进行梯度洗脱, 流速为0.4 mL/min, 采集210 nm色谱图进行样品初筛。GC-MS采用DB-5MS毛细管色谱柱(30 m×0.25 mm×0.25 μm)分离, 程序升温条件为: 初始温度150 ℃(1 min), 以8 ℃/min升至250 ℃(5 min), 12 ℃/min升至280 ℃(15 min), 选择EI离子源, 溶剂延迟2 min, 质谱扫描50~600 amu。结果 本方法能够在23 min内快速检测安神类保健食品中的新型非法添加药物, 先经UPLC分析样品发现可疑色谱峰, 再运用气质联用技术确证为一种新型非法添加药物盐酸氟桂利嗪。结论 该方法快速、简便、准确, 为保健食品中新型非法添加药物的检测提供了研究思路和参考。
Objective To establish a method of ultra performance liquid chromatography and gas chromatography-mass spectrometry for determination and confirmation of new illegal drug added in sleep-improving health-care foods. Method The samples were extracted through solvent ultrasonic extraction or the liquid-liquid extraction and tested by UPLC. In the UPLC method, ZORBAX SB-C18 column (2.1×150 mm, 1.8 μm)was used with the mobile phase of acetonitrile and 0.1% phosphoric acid for linear gradient elution. The flow rate was 0.4 mL/min. The detection wave lengths were 210 nm for preliminary screening. The analytical capillary column of GC-MS was DB-5MS (30 m×0.25 mm×0.25 μm). The temperature programming was as follows: the initial temperature was set at 150 ℃ (1 min); then raised to 250 ℃(5 min) with heating speed of 8 ℃/min, and to 280 ℃ (15 min) with heating speed of 12 ℃/min. The EI ion source was selected and the solvent delayed by 2 min. The MS scanning was set at the range of 50~600 amu. Results New illegal additives in sleep-improving health-care foods could be effectively detected within 23 min. Through analyzing by UPLC, a suspicious chromatographic peak was detected and then was confirmed to be a new kind of illegal additive flunarizine hydrochloride by GC-MS method. Conclusion The method is rapid, simple and accurate, which provides research mentality and reference for the determination of new illegal additive in health foods.
标题：安神类保健食品中新型非法添加药物的检测研究
英文标题：Study on determination of new illegal additives in sleep-improving health-care foods
作者：
林芳 陕西省食品药品检验所
王一欣 陕西省食品药品检验所
李涛 陕西省食品药品检验所
刘海静 陕西省食品药品检验所
袁磊 陕西省食品药品检验所
中文关键词:保健食品,新型非法添加物,盐酸氟桂利嗪,气相色谱-质谱法,超高效液相色谱法,
英文关键词:health foods,new illegally additives,flunarizine hydrochloride,gas chromatography-mass spectrometer,ultra performance liquid chromatography,
发表日期：2016-01-25
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