安神类保健食品中新型非法添加药物的检测研究

Study on determination of new illegal additives in sleep-improving health-care foods

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

中文摘要:

      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。

英文摘要:

      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.