分析化学Issue(12)：1759-1766,8.DOI:10.11895/j.issn.0253-3820.140729
阳离子交换在线固相萃取/液相色谱-串联质谱法检测牛奶中14种磺胺药物残留
Determination of 14 Sulfonamides Residue in Milk by On-line Solid Phase Extraction in Cation Exchange Mode/Liquid Chromatography-Tandem Mass Spectrometry
摘要
Abstract
To determine the residue of 14 sulfonamides in milk, a high performance liquid chromatography-tandem mass spectrometry ( HPLC-MS/MS ) method with on-line soild phase extraction ( SPE ) in cation exchange mode was established. 5 g of milk was extracted with 15 mL acetonitrile. Then the extraction was evaporated by 50 ℃ nitrogen and dissolved by 1. 00 mL 0. 2% formic acid. The dissolution was enriched and purified by MS/MS cation exchange on-line SPE column on a double ternary liquid chromatography, and eluted by the mixed solution of 2% ammonia methanol and 0. 2% formic acid (50:50, V/V). The compounds were separated by an octadecyl silica bonded column and determined by the tandem mass spectrometry. The results showed that the linearity of 14 sulfonamides was good in the range of 0 . 1–10 μg/kg ( r≥0 . 9995 ) . <br> The LOD of the method was 0. 05 μg/kg, while the LOQ was 0. 1 μg/kg. The recoveries of the 14 sulfonamides were in the range of 60 %-90 %, while the inter-batch and intra-batch RSDs were all lower than 10%. The method was proved to be more convenient, economical and stable than the traditional SPE column method.关键词
在线固相萃取/阳离子交换/双三元液相色谱-串联质谱法/磺胺类药物/牛奶Key words
On-line solid phase extraction/Cation exchange/Double ternary liquid chromatography-tandem mass spectrometry/Sulfonamides/Milk引用本文复制引用
顾欣,吴剑平,张鑫,李丹妮,严凤,周悦榕..阳离子交换在线固相萃取/液相色谱-串联质谱法检测牛奶中14种磺胺药物残留[J].分析化学,2014,(12):1759-1766,8.基金项目
本文系国家公益性行业(农业)科研专项(No.20120323)资金资助@@@@This work was supported by the Special Fund for Agro-scientific Research in the Public Interest ( No.201203023) （农业）
