超高效液相色谱-串联质谱法快速测定沉积物中11种藻毒素

Rapid Determination of 11 Algal Toxins in Sediments by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)快速测定沉积物中11种藻毒素的方法。沉积物经冷冻干燥、粉碎过筛,用0.1 mol/L EDTA-Na4P2O7溶液涡旋超声提取,经HLB固相萃取小柱净化后,用甲醇-0.2%甲酸洗脱、浓缩并氮吹定容至1 m L。经Waters BEH C18色谱小柱,以乙腈-0.2%甲酸水溶液为流动相,梯度洗脱分离后,在电喷雾正离子模式下,以超高效液相色谱-串联质谱多级监测模式(MRM)外标法进行定性定量分析。结果表明:沉积物中11种藻毒素的检出限为1.0~5.0 ng/kg。对同一环境样品进行了0.1、1.0、4.0μg/kg不同水平的加标回收试验,平均回收率为70.3%~112.5%,相对标准偏差(RSD)为2.2%~9.3%。该方法快速、灵敏、准确,可应用于沉积物中11种藻毒素的快速监测。

A method was established for the rapid determination of 11 algal toxins in sediments by ultra performance liquid chromatography - tandem mass spectrometry.Firstly,the sample was freezingly dried out,and then sieved,followed by purification with 0.1 mol/L EDTA-Na4P2O7 solution and HLB solid phase extraction column,elution with methanol-0.2% formic acid,and finally concentrated and mixed with nitrogen to 1 mL.The separation of the analyte was performed on a Waters BEH C18 chromatographic column with acetonitrile -0.2% formic acid solution as mobile phase by gradient elution.The sample was analyzed by ultra performance liquid chromatography-tandem mass spectrometry in positive ions electrospray mode under multi-stage monitoring mode （MRM）,and quantified by external standard method.The results showed that the detection limits for 11 algal toxins in sediment were in the range of 1.0-5.0 ng/kg.The average recoveries for the same environmental samples at three spiked concentrations of 0.1,1.0,4.0 μg/kg were in the range of 70.3%-112.5% with relative standard deviations of 2.2%-9.3%.The method was rapid,sensitive and accurate,and could be effectively applied in the rapid monitoring of 11 algal toxins in sediments.A method was established for the rapid determination of 11 algal toxins in sediments by ultra performance liquid chromatography - tandem mass spectrometry.Firstly,the sample was freezingly dried out,and then sieved,followed by purification with 0.1 mol/L EDTA-Na4P2O7 solution and HLB solid phase extraction column,elution with methanol-0.2% formic acid,and finally concentrated and mixed with nitrogen to 1 mL.The separation of the analyte was performed on a Waters BEH C18 chromatographic column with acetonitrile -0.2% formic acid solution as mobile phase by gradient elution.The sample was analyzed by ultra performance liquid chromatography-tandem mass spectrometry in positive ions electrospray mode under multi-stage monitoring mode （MRM）,and quantified by external standard method.The results showed that the detection limits for 11 algal toxins in sediment were in the range of 1.0-5.0 ng/kg.The average recoveries for the same environmental samples at three spiked concentrations of 0.1,1.0,4.0 μg/kg were in the range of 70.3%-112.5% with relative standard deviations of 2.2%-9.3%.The method was rapid,sensitive and accurate,and could be effectively applied in the rapid monitoring of 11 algal toxins in sediments.A method was established for the rapid determination of 11 algal toxins in sediments by ultra performance liquid chromatography - tandem mass spectrometry.Firstly,the sample was freezingly dried out,and then sieved,followed by purification with 0.1 mol/L EDTA-Na4P2O7 solution and HLB solid phase extraction column,elution with methanol-0.2% formic acid,and finally concentrated and mixed with nitrogen to 1 mL.The separation of the analyte was performed on a Waters BEH C18 chromatographic column with acetonitrile -0.2% formic acid solution as mobile phase by gradient elution.The sample was analyzed by ultra performance liquid chromatography-tandem mass spectrometry in positive ions electrospray mode under multi-stage monitoring mode （MRM）,and quantified by external standard method.The results showed that the detection limits for 11 algal toxins in sediment were in the range of 1.0-5.0 ng/kg.The average recoveries for the same environmental samples at three spiked concentrations of 0.1,1.0,4.0 μg/kg were in the range of 70.3%-112.5% with relative standard deviations of 2.2%-9.3%.The method was rapid,sensitive and accurate,and could be effectively applied in the rapid monitoring of 11 algal toxins in sediments.