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建立了一种同时定性和定量的超高效液相色谱串联质谱法(UPLC-MS/MS)来测定鲤(Cyprinuscarpio)血浆中磺胺间甲氧嘧啶(SMM)的血浆蛋白结合率。血浆样品采用乙腈提取,正己烷脱脂净化。提取液选用BEHC18(1.7μm,50mm×2.1mm)色谱柱分离,酸化的乙酸铵水溶液/乙腈梯度洗脱,电喷雾-多反应监测正离子模式定量定性分析。本方法线性范围为0.5～200ng/mL,r2≥0.998。添加水平为10、200、2000μg/L时,平均回收率在76.3%～90.3%之间,相对标准偏差均低于15%,最低检测限和定量限分别为0.2μg/L和0.5μg/L。20℃下,SMM在鲤中的血浆蛋白结合率为20.9%,达到平衡的时间为40h。本方法可快速、灵敏检测鲤血浆中磺胺间甲氧嘧啶含量,为研究磺胺间甲氧嘧啶的药理和药效及其在水产品中药物残留代谢规律提供了技术支持。
A simultaneous, qualitative and quantitative ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) was developed to determine the plasma protein binding of sulfamonomethoxine (SMM) in the plasma of Cyprinus carpio. Plasma samples were extracted with acetonitrile and defatted with n-hexane. The extracts were separated on a BEHC18 (1.7μm, 50mm × 2.1mm) column, acidified aqueous ammonium acetate / acetonitrile gradient, and electrosprayed to multiple reaction monitored positive ion mode. The linear range of this method is 0.5 ~ 200ng / mL, r2≥0.998. The average recovery was between 76.3% and 90.3% with the addition levels of 10,200,2000μg / L, and the relative standard deviations were all less than 15%. The minimum and maximum limits of detection were 0.2μg / L and 0.5μg / L, respectively . The plasma protein binding rate of SMM in carp was 20.9% at 20 ℃, and the equilibrium time was 40h. The method can rapidly and sensitively detect the content of sulfamethoxine in the plasma of the carp, and provides technical support for studying the pharmacology and efficacy of the sulfadimethoxine and the law of residual drug metabolism in aquatic products.