高效液相色谱-串联质谱法检测虾中9种磺胺类药物的残留(1)
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[摘要] 目的：建立虾中9种磺胺类抗生素残留的高效液相色谱-串联质谱同时测定方法。方法：样品经乙腈提取，经脱脂、净化、浓缩后，以A相为甲醇、B相0.50 mmol/L乙酸铵溶液为流动相，采用HPLC-MS/MS多反应监测(MRM)正离子模式测定。结果：9种磺胺类药物在0～100 ng/ml范围内线性关系良好(γ>0.999 0)，加标回收率为75.3%～95.6%，相对标准偏差(RSD)为4.5%～13.5%。结论：该方法准确、可靠、灵敏度好，适用于磺胺类药物残留的检测。
[关键词] 高效液相色谱-质谱法；磺胺；药物残留；虾
[中图分类号] R92[文献标识码] C[文章编号] 1674-4721(2011)08(b)-060-03
Simultaneous determination of 9 sulfonamides residues in shrimps by high performance liquid chromatography-tandem mass spectrometry
BAI Lili1, DAI Hua2, LIN Zhengfeng3
1.Department of Pharmacy, Hainan Medical University, Hainan Province, Haikou 571101, China; 2.School of Public Health, Hainan Medical University, Hainan Province, Haikou 571101, China; 3.Entry-Exit Inspection and Quarantine Bureau, Hainan Province, Haikou 570311, China
[Abstract] Objective: To develop the method for the simultaneous determination of 9 sulfonamides (SAs) residues in shrimps by high performance liquid chromatography and tandem mass spectrometry (HPLC-MS/MS). Methods: The sample was extracted with acetonitrile, defatted and purified and then concentrated by evaporation. The 9 analytes were separated with a mobile phase composed of methanol and 0.50 mmol/L aqueous ammonium acetate solution. The mass spectrometer was operated using multiple reaction monitoring (MRM). Results: The 9 drugs showed good linear correlation in the range of 0-100 ng/ml (γ>0.999 0). The average recovery rate was 75.3% to 95.6% at two concentration levels. The relative standard deviation was 4.5% to 13.5%. Conclusion: The results indicate that the HPLC-MS/MS assay is accurate, reliable, and sensitive, thus it is suitable for the determination of SAs in aquatic products.
[Key words] High performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS); Sulfonamides; Drug residue; Shrimp
磺胺类药物(SAs)是具有对氨基苯磺酰胺结构的一类药物的总称，是常用的广谱抗生素。因其具有抗菌谱广、高效、低毒和价格低廉等特点，在水产养殖中被广泛使用。人类经常食用有磺胺类药物残留的动物源性食品，就可能引起磺胺类药物在体内的逐渐累积，其危害性主要表现为细菌耐药性、过敏、造血紊乱、致癌作用以及激素样作用等[1-2]。目前中国、欧盟、美国、日本等均将磺胺类药物列为动物饲养过程中限制使用的药物，其最大残余限量一般为50～100 μg/kg。目前，用于抗生素的检测方法有高效液相色谱法(HPLC)、酶联免疫分析法(ELISA)、气相色谱法(GC)、高效毛细管电泳法(HPCE)、液相色谱-质谱法(HPLC-MS/MS)等方法[3-5] ......
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