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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-C_(18)(2.1×150 mm,1.8μm)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 m L/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×0.25mm×0.25μm)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 ultra-performance liquid chromatography (UPLC) and gas chromatography-mass spectrometry (GC-MS) for the detection and confirmation of new illicit drugs added to soothe the nerves health food. Methods The samples were extracted by solvent ultrasonic or liquid-liquid extraction and determined by UPLC. UPLC was separated on a ZORBAX SB-C 18 (2.1 × 150 mm, 1.8 μm) column using acetonitrile and 0.1% phosphoric acid as the mobile phase at a flow rate of 0.4 mL / min. A 210 nm chromatogram Sample screening. GC-MS was separated on a DB-5MS capillary column (30 m × 0.25 mm × 0.25 μm). The temperature programmed conditions were as follows: the initial temperature was 150 ° C for 1 min, and the temperature was raised to 250 ° C for 5 min at 8 ° C / The temperature was raised from 12 ° C / min to 280 ° C (15 min). The EI ion source was selected and the solvent was delayed for 2 min. The mass spectrum was scanned for 50-600 amu. Results The method was able to rapidly detect new illicit drugs in the soothe class health food within 23 min. The samples were analyzed by UPLC for suspicious chromatographic peaks and then identified by GC / MS as a new type of illicit drug, flunarizine hydrochloride . Conclusion The method is rapid, simple and accurate, which provides a research idea and reference for the detection of new illicitly added drugs in health food.