UPLC-MS/MS测定减肥食品中8种非法添加化学成分

Determination of 8 Illegal Added Chemical Composition in the Slimming Health Food by UPLC-MS/MS

关键词:  UPLC-MS/MS  减肥食品  化学成分  非法添加

Key words:  UPLC-MS/MS  slimming health food  chemical composition  illegally added

摘要:

目的 建立一种简便有效检测减肥食品中非法添加化学成分的UPLC-MS/MS检测方法。方法 采用UPLC-MS/MS法，以Eclipse Plus C₁₈（2.1 mm×50 mm，1.8 μm）色谱柱分离，串联四级杆质谱仪检测，多反应监测模式进行定性定量分析，以流动相A（0.02 mol·L^-1乙酸铵水溶液）-B（甲醇）进行梯度洗脱；柱温：40℃；流速：0.3 mL·min^-1，进样量2 μL。样品以甲醇为溶剂超声提取，快速定性定量检测非法添加在减肥食品中的麻黄碱、咖啡因、呋塞米、芬氟拉明、酚酞、N-单去甲基西布曲明、N，N-双去甲基西布曲明、西布曲明8种化学成分。结果 8种减肥类化学成分质谱检测的线性范围宽，相关性R² ≥ 0.995；方法检测限为0.042~0.175 μg·mL^-1，定量限为0.126~0.525 μg·mL^-1，方法精密度RSD（n=6）为1.7%~4.7%；3个浓度水平的平均回收率为90.3%~105.1%。结论 本方法专属性强、操作简单、方便快捷，可作为食品中非法添加减肥类化学成分的有效检测方法。

Abstract:

OBJECTIVE To develop a UPLC-MS/MS method to determine illegal chemical composition added into the slimming health food. METHODS The analysis was performed by a UPLC-MS/MS system with Eclipse Plus C₁₈(2.1 mm×50 mm, 1.8 μm) column, with 0.02 mol·L^-1 acetic acid (A)-methanol (B) as mobile phase by gradient elution at a flow rate of 0.3 mL·min^-1, and the column temperature was 40℃. Multiple-reaction monitoring (MRM) was performed to identify and quantify 8 chemical drugs, including ephedrine hydrochloride, caffeine, furosemide, fenfluramine, phenolphthalein, N-single demethylated sibutramine, N,N-didesmethylsibutramine and sibutramine. RESULTS A good resolution of 8 kinds of chemical drugs were obtained under this UPLC-MS/MS condition. Eight linear calibration curves were obtained with R² ≥ 0.996 7. The limits of qualitation and quantitation were in the range of 0.042-0.175 μg·mL^-1 and 0.126-0.525 μg·mL^-1. The precision of the method were showed by RSD (n=6) ranged from 1.7% to 4.7%. The average recoveries (n=6) were in the range of 90.3% to 105.1% at three concentrations levels. CONCLUSION The method is simple, accurate, and highly sensitive, which can be used for the determination of illegally added chemical drugs in slimming health foods.