Captiva EMR-Lipid小柱净化-超高效液相色谱-串联质谱法快速测定水产品中五氯酚钠残留

Rapid determination of sodium pentachlorophenol in aquatic products by captiva EMR-lipid soild phase extraction-ultra performance liquid chromatography-tandem mass spectrometry

本研究建立了一种基于Captiva EMR-Lipid小柱净化结合高效液相色谱-串联质谱技术(LC-MS/MS)快速分析多种水产品基质中五氯酚钠残留的方法。样品经1%乙酸乙腈溶液(v/v)提取,Captiva EMR-Lipid小柱净化后采用LC-MS/MS方法进行检测。选择ZORBAX RRHD Eclipse Plus C_(18)色谱柱作为分析柱,甲醇和5 mmol/L甲酸铵水溶液为流动相进行梯度洗脱,多反应监测负离子模式扫描,同位素内标法定量。结果表明,五氯酚钠在相关范围内线性关系良好,相关系数r不低于0.99,本研究方法在缢蛏(Sinonovacula constricta)、罗氏沼虾(Macrobrachium rosenbergii)、大口黑鲈(Micropterus salmoides)、中华鳖(Trionyx Sinensis)、大黄鱼(Larimichthys crocea)和青蟹(Scylla)样品中的定量限均为0.5μg/kg,基质加标回收率范围为89.6%~103.0%,相对标准偏差为4.39%~12.20%。该方法操作简便,测定结果准确、可靠,适用于水产品中五氯酚钠残留的快速测定。

An high performance liquid chromatography-tandem mass spectrometry(LC-MS/MS)with Captiva EMR-lipid pretreatment technique was established for the simultaneous analysis of sodium pentachlorophenol in aquatic products.Each sample was firstly extracted with acetonitrile(1%acetic acid,v/v),then purified with Captiva EMR-lipid filtration column,and finally detected by LC-MS/MS.The samples were analyzed on the ZORBAX RRHD Eclipse Plus C_(18) column using methanol and 5 mmol/L ammonium formate as mobile phase.The quantitative determination for the analytes was carried out under the multiple reaction monitoring mode with negative electrospray ionization by using isotope internal standard method.Results showed that there were good linear relationships for analytes in the corresponding concentration ranges,along with correlation coefficient≥0.99.The limits of quantification for this method in Sinonovacula constrzcta,Macrobrachium rosewere,Micropterus salmoides,Trionyx sinensis,Larimichthys crocea and Scylla samples were all 0.5μg/kg.The average spiked recoveries were between 89.6%and 103.0%and the relative standard deviations of 4.39%-12.20%.With simple operation and high accuracy,this method is suitable for rapid determination of sodium pentachlorophenol in aquatic products.