减肥保健食品中非法添加酚酞和西布曲明的同时检测

doi:10.7506/spkx1002-6300-201004035

食品科学 ›› 2010, Vol. 31 ›› Issue (4): 156-160.doi: 10.7506/spkx1002-6300-201004035

减肥保健食品中非法添加酚酞和西布曲明的同时检测

马微^1,2，王海波²，马强³，付丽⁴，李立³，唐英章^3,*

1.东宁出入境检验检疫局 2.中国农业大学 3.中国检验检疫科学研究院 4.郑州牧业工程高等学校

收稿日期:2009-05-14 修回日期:2009-11-12 出版日期:2010-02-15 发布日期:2010-12-29
通讯作者: 马微 E-mail:mawei1599@126.com
基金资助:
“十一五”国家科技支撑计划项目(2006BAD27B02)

Simultaneous Determination of Phenolphthalein and Sibutramine Illegally Added to Weight Loss Functional Foods

MA Wei1,2，WANG Hai-bo2，MA Qiang3，FU Li4，LI Li3，TANG Ying-zhang3,*

1. Dongning Entry-Exit Inspection and Quarantine Bureau, Dongning 157200, China；2. China Agricultural University, Beijing
100083, China；3. Chinese Academy of Inspection and Quarantine, Beijing 100123, China；4. Zhengzhou College of Animal
Husbandry Engineering, Zhengzhou 450011, China

Received:2009-05-14 Revised:2009-11-12 Online:2010-02-15 Published:2010-12-29
Contact: MA Wei E-mail:mawei1599@126.com

摘要/Abstract

摘要：

目的：建立测定减肥保健食品中非法添加酚酞和西布曲明的高效液相色谱- 串联质谱分析方法，并通过研究其质谱特征，推测其裂解途径。方法：减肥咖啡、减肥茶、减肥胶囊、苹果醋咀嚼片、减肥蛋白素等不同类型的减肥保健食品经超声波辅助提取15min，以Waters Atlantis T3 柱(150mm × 2.1mm，3μm)分离后，进行HPLCMS/MS 多反应监测模式下的定性及定量分析。结果：酚酞在2.5～500μg/L 的范围内呈良好的线性关系，相关系数为0.9992；西布曲明在0.15～500μg/L 的范围内呈良好的线性关系，相关系数为0.9996。在低、中、高3 个添加水平范围内的平均回收率为82.3%～103.6%；日内精密度均小于5%，日间精密度均小于8%。在检测的20 种样品中，检出含有西布曲明的样品13 个，检出率为65%；含有酚酞的样品9 个，检出率为45%。结论：本方法分析速度快、灵敏度高、回收率好，可用于不同减肥保健食品中非法添加酚酞和西布曲明的同时检测。

关键词: 减肥保健食品, 高效液相色谱- 串联质谱, 酚酞, 西布曲明, 质谱裂解途径

Abstract:

A simple and rapid method using high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) was developed for the simultaneous determination of phenolphthalein and sibutramine illegally added to weigh loss functional foods. Along with this, mass spectral fragmentation pathways of the above analytes were elucidated. In the method, various samples, including weight loss coffee, tea, capsule and albumin as well as apple vinegar chewing tablets were extracted for 15 minutes using methanol with the assistance of ultrasonic. Qualitative and quantitative analysis was carried out for 20 samples in the MRM mode following chromatographic separation on a Waters Atlantis T3 (150 mm × 2.1 mm, 3μm) column. Linear ranges for phenolphthalein and sibutramine detected by the method were 2.5 － 500μg/L and 0.15 － 500μg/L, and corresponding correlation coefficients 0.9992 and 0.9996, respectively. Mean recoveries for both analytes in aforementioned 5 types of weight loss functional foods at three spike levels (low, medium and high) were within the range of 82.3%－103.6% (n = 6), with intraday precision RSDs less than 5% and inter-day precision RSDs less than 8%. Sibutramine was detected in 13 of 20 samples, and namely the detection ratio was 65%. Phenolphthalein was detected in 9 of 20 samples and namely the detection ratio was 45%. This method is characterized by rapidity, high sensitivity and recovery, and good reliability, thereby providing a robust approach for the determination of phenolphthalein and sibutramine illegally added to weight loss functional foods.

Key words: weight loss functional food, high performance liquid chromatography tandem mass spectrometry (HPLC-MS/ MS), phenolphthalein, sibutramine, mass spectral fragmentation pathway

中图分类号:

TS201.6

马微1,2，王海波2，马强3，付丽4，李立3，唐英章3,*. 减肥保健食品中非法添加酚酞和西布曲明的同时检测[J]. 食品科学, 2010, 31(4): 156-160.

MA Wei1,2，WANG Hai-bo2，MA Qiang3，FU Li4，LI Li3，TANG Ying-zhang3,*. Simultaneous Determination of Phenolphthalein and Sibutramine Illegally Added to Weight Loss Functional Foods[J]. FOOD SCIENCE, 2010, 31(4): 156-160.

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减肥保健食品中非法添加酚酞和西布曲明的同时检测

Simultaneous Determination of Phenolphthalein and Sibutramine Illegally Added to Weight Loss Functional Foods

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