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机构地区:[1]大连市水产技术推广总站,辽宁大连116023 [2]大连理工大学,辽宁大连116023
出 处:《现代科学仪器》2013年第1期143-145,148,共4页Modern Scientific Instruments
摘 要:优化了液相色谱-串联质谱法测定水产品中孔雀石绿和无色孔雀石绿残留量的检测方法。样品经匀浆、萃取、净化和浓缩后,用2mL的乙腈-5mmol/L乙酸铵溶液(1+1)定容,采用液相色谱-三重四级杆串联质谱仪、多反应监测扫描模式(MRM)检测和同位素内标法定量。孔雀石绿和无色孔雀石绿检测的线性范围为0.25~10.0ng/mL,检出限均为0.50μg/kg。在加标量为2.50μg/kg时,样品加标平均回收率分别为98.1%和93.4%,相对标准偏差(RSD)小于10%,满足水产品中孔雀石绿和无色孔雀石绿残留量的检测要求。In this study,we optimized a high performance liquid chromatography-tandem mass spectrometric(HPLC-MS/MS)method for determining malachite green and leumalachite green in fishery products.Samples were subjected to homogenate,extraction,purification,concentration and constant volume prior to HPLC-MS/MS analysis.The analysis was carried out in the multi-reaction monitoring(MRM) mode and internal standard isotope dilution method was used for quantification.Calibration curves for the analytes exhibited good linearity over the concentration range from 0.5 to 10.0 ng/mL and their limits of quantification were all 0.50μg/kg.Average recoveries for them were 98.1% 93.4% respectively with amounts of standard addition of 2.50μg/kg,And relative standard deviations(RSDs) was less than 10%.The method can meet the requirements of detection for malachite green and leumalachite green in fishery products.
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