建立了一种专属、灵敏的同时测定减肥保健食品中非法添加的药物利莫那班和奥利司他的高效液相色谱-串联质谱分析方法.不同类型的减肥保健食品经加速溶剂萃取后,用甲醇和10 mmol/L 乙酸铵水溶液作流动相,采用梯度洗脱方式以Waters Atlantis T3色谱柱(150 mm×2.1 mm, 3 μm)分离,以电喷雾离子源正离子检测方式进行质谱分析.实验结果表明,利莫那班和奥利司他的方法检出限为0.5 mg/kg;在0.5～100 μg/L 范围内呈良好的线性关系,相关系数分别为 0.9989 和 0.9994;在2, 5, 10 mg/kg 3个添加水平范围内的平均回收率为80.5% ～102.1% ;日内精密度均小于6% ,日间精密度均小于8% .同时研究了这两种药物的质谱特征,推测了其质谱裂解途径.本方法灵敏度高,重现性好,可用于不同类型减肥保健食品中非法添加的奥利司他和利莫那班的检测.
A sensitive and selective analytical method based on high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) has been developed for the simultaneous determination of rimonabant and orlistat in weight-loss functional foods. After the foods were extracted under accelerated solvent extraction, the HPLC separation was performed on a Waters Atlantis T3 column (150 mm × 2.1 mm, 3 μm) with a linear gradient elution program of methanol and 10 mmol/L ammonium acetate as the mobile phase. Electrospray ionization was applied and operated in the positive ion mode. The results showed that the limits of detection for the rimonabant and orlistat were 0.5 mg/kg. The calibration curves showed good linearities for rimonabant and orlistat in the range of 0.5-100 μg/L, and the correlative coefficients were 0.9989 and 0.9994, respectively. The mean recoveries at the 3 spiked levels (2, 5, 10 mg/kg) were 80.5% -102.1% with the intra-day precision less than 6% and the inter-day precision less than 8% . The work studied the mass spectrum characterization of the 2 drugs and speculated on the fragmentation pathways. The method is sensitive, reproducible and adapts to the determination of rimonabant and orlistat in different weight-loss functional foods.
参考文献
| [1] | Ballinger A,Peikin S R.Eur J Pharmacol,2002,440:109 |
| [2] | Tonstad S.Nutrition,Metabolism & Cardiovascular Diseases,2006,16:156 |
| [3] | Zi M,Li X X.Adverse Drug Reactions Journal (訾梅,李祥霞.药物不良反应杂志),2007,9(3):182 |
| [4] | Que B.Chinese Journal of Cardiovascular Review (阙斌.中国心血管病研究),2007,5(10):769 |
| [5] | McCulloch M,Zhou X,Xu Y,et al.J Chromatogr B,2008,863:258 |
| [6] | Delyle S G,Abe E,Devillier P,et al.J Chromatogr B,2008,872:115 |
| [7] | Wieboldt R,Campbell D A,Henion J.J Chromatogr B,1998,708:121 |
| [8] | Bennett P K,Li Y T,Edom R,et al.J Mass Spectrom,1997,32(7):739 |
| [9] | Garland W A.Report MS 32.Nutley,NJ,USA:Hoffman La Roche,1990:178 |
| [10] | Mohammadi A,Haririan I,Rezanour N,et al.J Chromatogr A,2006,1116:153 |
| [11] | Xiao S,Zhu X L,Chen B,et al.Journal of Hygiene Research (肖松,朱小兰,陈波,等.卫生研究),2006,35(3):355 |
| [12] | Ye M L,Zhu Y.Modern Scientific Instruments (叶明立,朱岩.现代科学仪器),2003(1):35 |
| [13] | Wang Y X,Xu X S.Journal of Instrumental Analysis (王宇晓,许学书.分析测试学报),2007,26(8):50 |
| [14] | Commission of the European Communities.2002/657/EC.[2002-08-14].http:/ /www.wetgiw.gov.pl/old/UE/prawo/02_657/e02657.pdf |
- 下载量()
- 访问量()
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%