SUN Yanchun, WANG Ying, DU Ningning, WU Song, MOU Zhenbo, TANG Shizhan

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        液相色譜串聯質譜測定磺胺間甲氧嘧啶與鯉魚血漿蛋白結合率
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        作者簡介:孫言春(1979-),男,助理研究員,博士研究生,主要從事水產品質量安全和環境研究。Email:sunyc2004@163.com 通訊作者:牟振波,研究員,研究方向為冷水魚養殖和水產品質量安全。Email: mouzhenbo@163.com

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        中國水產科學研究院與黑龍江水產研究所基本科研專項(2012A1004,2011 HSYZX-HJ)


        Determination of protein binding of Sulfamonomethoxine with common carp (Cyprinus carpio) plasma by liquid chromatography-tandem mass spectrometry
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          摘要:建立了一種同時定性和定量的超高效液相色譜串聯質譜法(UPLC-MS/MS)來測定鯉(Cyprinus carpio血漿中磺胺間甲氧嘧啶(SMM)的血漿蛋白結合率。血漿樣品采用乙腈提取,正己烷脫脂凈化。提取液選用BEH C181.7 μm,50 mm×2.1 mm)色譜柱分離,酸化的乙酸銨水溶液/乙腈梯度洗脫,電噴霧-多反應監測正離子模式定量定性分析。本方法線性范圍為0.5 ~200 ng/mL,r20.998。添加水平為10、200、2 000 µg/L時,平均回收率在76.3% ~90.3 %之間,相對標準偏差均低于15%,最低檢測限和定量限分別為0.2 μg/L0.5 μg/L。20 ℃下,SMM在鯉魚中的血漿蛋白結合率為20.9%,達到平衡的時間為40 h。本方法可快速、靈敏檢測鯉血漿中磺胺間甲氧嘧啶含量,為研究磺胺間甲氧嘧啶的藥理和藥效及其在水產品中藥物殘留代謝規律提供了技術支持。[中國漁業質量與標準,2012,2(4):81-85]

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          Abstract: A quantitative and qualitative method of ultra-performance liquid chromatography coupled to triple quadruple tandem mass spectrometry UPLCTM-MS/MS has been developed for the rapid and sensitive determination of the protein binding of sulfamonomethoxine(SMM) with common carp (Cyprinus carpio) plasma. After extraction with acetonitrile and defatted with n-hexane, the plasma extract was performed with the C18 columnBEH C18 1.7 μm, 2.1 mm × 50 mm, and then separated by gradient elution using ammonium acetate/formic acid solution and acetonitrile. Mass spectrometric determination was carried out with an electrospray ionization interfaceESIin positive ion mode with multiple reactions monitoring modeMRM. The calibration curve ranging from 0.5 to 200 ng/mL in fluent phase solvent was used to establish instrument response, with relative standard coefficient beyond 0.998. The method was validated by analysis of nine replicate plasma samples fortified with three kinds of concentration levels of 2 μg/L,20 μg/L and 100 μg/L SMM, respectively. Depending on the biological matrix and analyte,relative standard deviations were below 15 %,with average recovery rates around 76.3 % to 90.3 % in spiked samples and the limit of detection LOD and quantification LOQ for the analyte were 0.25 μg/kg and 0.5 μg/kg using 1.0mL sample, respectively,and the precision and recovery were all satisfying. Finally, the method was successfully used to determinate the protein binding of common carp plasma with SMM under 20 by equilibrium dialysis method, and the equilibrium time was 40 h and the rate of protein binding was 20.9%.[Chinese Fishery Quality and Standards, 2012, 24):00-00]

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        孫言春,王瑛,杜寧寧,等.液相色譜串聯質譜測定磺胺間甲氧嘧啶與鯉魚血漿蛋白結合率[J].中國漁業質量與標準,2012,2(4):81-85.

        SUN Yanchun, 復制

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        • 最后修改日期:2013-01-25
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