| 引用本文: | 裘一婧,曹王丽,方玲.UPLC-MS/MS测定减肥食品中8种非法添加化学成分[J].中国现代应用药学,2017,34(10):1441-1446. |
| QIU Yijing,CAO Wangli,FANG Ling.Determination of 8 Illegal Added Chemical Composition in the Slimming Health Food by UPLC-MS/MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2017,34(10):1441-1446. |
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| 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。 |
| 关键词: UPLC-MS/MS 减肥食品 化学成分 非法添加 |
| DOI：10.13748/j.cnki.issn1007-7693.2017.10.017 |
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| Determination of 8 Illegal Added Chemical Composition in the Slimming Health Food by UPLC-MS/MS |
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QIU Yijing1, CAO Wangli2, FANG Ling2,3
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1.Hangzhou Institute for Food and Drug Control, Hangzhou 310052, China;2.Zhejiang CONBA Pharmaceutical Co., Ltd., Hangzhou 310052, China;3.Zhejiang Key Laboratory of Traditional Chinese Medicine Pharmaceutical Technology, Hangzhou 310052, China
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| 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. |
| Key words: UPLC-MS/MS slimming health food chemical composition illegally added |
