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

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。

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

A method was established for the rapid deternmination 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 C1s 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.