84批减肥类保健食品中非法添加化学物质的数据分析

Data Analysis of Illegally Adding Chemical Substances in 84 Batches of Slimming Health Foods

关键词:  减肥类保健食品  非法添加化学物质  液-质联用  盐酸西布曲明  酚酞  呋塞米  分布范围

Key words:  slimming health foods  illegally added chemicals  HPLC-MS/MS  sibutramine hydrochloride  phenolphthalein  furosemide  distribution range

摘要:

目的 采用液-质联用方法，检测减肥类保健食品中可能违法添加的7种化学物质（盐酸芬氟拉明、酚酞、咖啡因、呋塞米、盐酸西布曲明、N，N-双去甲基西布曲明、N-单去甲基西布曲明），对84批减肥类保健食品的数据进行分析，绘制非法添加化学物质的每次摄入量分布图，为监管部门提供数据参考。方法 HPLC-MS/MS联用，Waters XBridge C₁₈色谱柱（4.6 mm×250 mm，5 μm）；以0.02 mol·L^-1醋酸铵溶液（含0.4%冰醋酸）-甲醇梯度洗脱，流速为0.3 mL·min^-1；ESI正负离子模式，一级、二级质谱全扫描，HPLC定量，HPLC-MS/MS定性。结果 84批样品中，有62批检出非法添加化学物质，分别为盐酸西布曲明、酚酞和呋塞米。每次摄入量分布图显示，在减肥类保健食品中，盐酸西布曲明的每次摄入量集中在0~10 mg和20~40 mg；酚酞的每次摄入量集中在0~10 mg，中位数为11.70 mg；呋塞米的每次摄入量集中在0~20 mg，中位数为12.01 mg。结论 目前，减肥类保健食品中非法添加的化学物质，以盐酸西布曲明、酚酞和呋塞米比较常见，其添加量的分布不均匀，安全隐患较大。

Abstract:

OBJECTIVE To detect 7 chemical substances(fenfluramine hydrochloride, phenolphthalein, caffeine, furosemide, sibutramine hydrochloride, N,N-bis-desmethylsibutramine and N-monodesmethylsibutramine) that may be illegally added in slimming health foods by HPLC-MS/MS, and to draw the distribution map of illegally added chemical substances, according to the data analysis results of 84 batches of slimming health foods tested, in order to provide data support of the regulatory authorities. METHODS HPLC-MS/MS was used with Waters XBridge C₁₈(4.6 mm×250 mm, 5 μm) as the column; eluted with a gradient of 0.02 mol·L^-1 ammonium acetate solution (containing 0.4% glacial acetic acid) and methanol. The flow rate was 0.3 mL·min^-1; ESI positive and negative ion mode, full-scale scanning of primary and secondary mass spectrometry were used. HPLC was used for quantitative, HPLC-MS/MS was used for qualitative. RESULTS Illegally added sibutramine hydrochloride, phenolphthalein and furosemide were found in 62 batches of the 84 batches. Distribution graph of intake per time showed that each intake of sibutramine hydrochloride was concentrated in 0-10 mg and 20-40 mg; each intake of phenolphthalein was concentrated in 0-10 mg, with a median of 11.70 mg; each intake of furosemide was concentrated in 0-20 mg, with a median of 12.01 mg. CONCLUSION At present, the illegally added chemical substances in slimming health foods are more common with sibutramine hydrochloride, phenolphthalein and furosemide, and the distribution of the added amount is not uniform. There are major security risks.