UPLC―MSMS测定水产品中孔雀石绿残留量控制图应用.docVIP

UPLC―MSMS测定水产品中孔雀石绿残留量控制图应用 　　摘要 通过优化前处理建立水产品中孔雀石绿残留量的UPLC-MS/MS测定方法，并应用控制图。样品经乙腈提取、固相萃取柱净化和浓缩，采用Zorbax Eclipse Plus C18色谱柱，以乙腈-乙酸铵缓冲液（5 mmol/L）为流动相，在ESI正离子模式下检测。通过对36批次孔雀石绿和46批次无色孔雀石绿加标回收率测试，经过数理统计，绘制孔雀石绿和无色孔雀石绿的回收率质量控制图，得出孔雀石绿的行动限为71.8%～121.9%，警告限为80.2%～113.6%；无色孔雀石绿的行动限为79.5%～129.0%，警告限为87.8%～120.7%。结果表明，质量控制图能直观有效地反映UPLC-MS/MS法测定水产品中孔雀石绿和无色孔雀石绿的分析质量变化趋势，确保检测结果准确可靠。 　　关键词 优化；控制图；孔雀石绿；水产品；超高效液相色谱-串联质谱法 　　中图分类号 TS207.7 文献标识码 A 文章编号 1007-5739（2017）20-0240-04 　　Application of Control Chart in Determination of Malachite Green Residues in Aquatic Products by UPLC-MS/MS 　　NI Jian-xiu CHEN Tao CHEN Gui-fang 　　（Nanjing Agricultural Products Quality Inspection of Jiangsu Province，Nanjing Jiangsu 210036） 　　Abstract A detection method of malachite green residues in aquatic products was established by UPLC-MS/MS，through the optimization of pretreatment extraction methods，and control chart was used.The samples were extracted with acetonitrile，purified by a solid-phase extraction column and concentrated，separated by using Zorbax Eclipse Plus C18 column with acetonitrile-ammonium acetate buffer（5 mmol/L） as the mobile phase and ESI positive ion mode detection.Recoveries of standard addition were tested for 36 batches of malachite green and 46 batches of leucomalachite green samples， and then mathematical statistics were used to work out the quality control chart，the action limits of malachite green were 71.8%-121.9%，the warning limits were 80.2%-113.6%；the action limits of leucomalachite green were 79.5%-129.0%，the warning limits were 87.8%-120.7%.It was indicated that the quality control chart could directly and effectively control the determination of malachite green in aquatic products with UPLC-MS/MS，and ensure the accurate and reliable detection result. 　　Key words optimization；control chart；malachite green；aquatic product；UPLC-MS/MS 　　孔雀石绿（malachite green，MG）是一?N三苯甲烷型绿色染料，曾因其廉价、高效的杀菌、杀寄生虫等性能而被用于水产养殖业，由于没有有效的替代品，孔雀石绿在水产养殖中的使用屡禁不止。孔雀石绿易被鱼体吸收并快速代谢为无色孔雀石绿（leucomalach