色谱Issue(8)：892-896,5.DOI:10.3724/SP.J.1123.2015.04008
超高效液相色谱-串联质谱法测定调制乳中3种磺胺类药物残留
Simultaneous determination of three sulfonamide residues in modified milk by ultra performance liquid chromatography-tandem mass spectrometry
程国栋 1吴小慧 1金珠 1张宇 1郝单 1仝面换 1高建军1
作者信息
- 1. 蒙牛乳业 马鞍山 有限公司，安徽 马鞍山 243000
- 折叠
摘要
Abstract
An ultra performance liquid chromatography-tandem mass spectrometry( UPLC-MS/MS)method for the residue determination of sulfadiazine,sulfamerazine and sulfamethazine in modified milk was established. The modified milk samples were extracted and their protein pre-cipitated with water( containing 1%( v/v)acetic acid)and methanol. Then they were purified with an HLB solid phase extraction cartridge. The separation was performed on an ACQUITY UPLC HSS T3 column(100 mm×2.1 mm,1.8 μm)with a gradient system of water(containing 0.1%(v/v)formic acid)and acetonitrile as mobile phases at a flow rate of 0.3 mL/min,and detected by the MS in ESI+ mode. Standard curves were drawn by using matrix standard addi-tion method,and the external standard method was used for quantitative analysis. The limits of quantification were 1 μg/kg. The calibration curves for the three sulfa drugs were linear in the mass concentration range of 1-100 μg/L with R2≥0.998. The recoveries at the levels of 1,2,10μg/kg fortified samples ranged from 76.5% to 101.9% with the relative standard deviations of 1.2%-12.4%. The method is simple, rapid, accurate, and its performance can meet the requirements of the domestic and international legislations. It is suitable for the detection of sulfonamide residues in modified milk.关键词
固相萃取/超高效液相色谱-串联质谱/磺胺类药物/调制乳Key words
solid phase extraction( SPE )/ultra performance liquid chromatography-tandem mass spectrometry( UPLC-MS/MS)/sulfonamides/modified milk分类
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程国栋,吴小慧,金珠,张宇,郝单,仝面换,高建军..超高效液相色谱-串联质谱法测定调制乳中3种磺胺类药物残留[J].色谱,2015,(8):892-896,5.
