引用本文:张蓓蓓,史震宇,吴仲夏,彭英,杨雪.加速溶剂萃取-固相萃取/超高效液相色谱-串联质谱法测定沉积物中5种微囊藻毒素[J].环境监控与预警,2018,10(2):19-22
ZHANG Bei-bei,SHI Zhen-yu, WU Zhong-xia, PENG Ying,YANG Xue.Simultaneous Determination of Five Microcystins in Sediment by Accelerated Solvent Extraction, Solid Phase Extraction and Ultra performance Liquid Chromatography Tandem Mass Spectrometry[J].Environmental Monitoring and Forewarning,2018,10(2):19-22
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加速溶剂萃取-固相萃取/超高效液相色谱-串联质谱法测定沉积物中5种微囊藻毒素
张蓓蓓,史震宇,吴仲夏,彭英,杨雪
国家环境保护地表水环境有机污染物监测分析重点实验室,江苏省环境监测中心,江苏 南京 210036
摘要:
建立了加速溶剂萃取-固相萃取/超高效液相色谱-串联质谱法同时测定沉积物中5种微囊藻毒素(MC-LR、MC-RR、MC-LW、MC-LF、MC-YR)的方法。选择甲醇-水(1∶4,V/V)为ASE萃取溶剂,萃取温度和萃取压力分别为80℃和13.1 MPa,固相萃取过程以HLB小柱为萃取柱,采用液相色谱-串联质谱分析。方法在5种微囊藻毒素质量浓度5~100 μg/L内线性良好(r>0.995),回收率为76.0%~118%,相对标准偏差为1.9%~12.0%,检出限为2~3 μg/kg,定量下限为8~12 μg/kg。该方法已用于西太湖沉积物的检测,具有较好的方法适用性。
关键词:  微囊藻毒素  超高效液相色谱-串联质谱  加速溶剂萃取  固相萃取  沉积物
DOI:
分类号:O657.7
文献标识码:B
基金项目:江苏省太湖水环境综合治理科研基金资助项目(TH2016301),江苏省环境监测基金资助项目(1413;1210)
Simultaneous Determination of Five Microcystins in Sediment by Accelerated Solvent Extraction, Solid Phase Extraction and Ultra performance Liquid Chromatography Tandem Mass Spectrometry
ZHANG Bei-bei,SHI Zhen-yu, WU Zhong-xia, PENG Ying,YANG Xue
State Environmental Protection Key Laboratory of Monitoring and Analysis for Organic Pollutants in Surface Water,Jiangsu Environmental Monitoring Center, Nanjing, Jiangsu 210036, China
Abstract:
An ultra-performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS)method was developed for the analysis of five microcystins (MC-LR、MC-RR、MC-LW、MC-LF、MC-YR) in sediment by accelerated solvent extraction(ASE)and solid phase extraction(SPE). The analytes were extracted by ASE using methanol/water ( 1∶4,by volume) as solution. The extraction temperature was 80℃ and the extraction pressure was 13.1 MPa . The extracts were enriched and purified by SPE with HLB column subsequently. The samples were finally analyzed by UPLC-MS/MS.The calibration curves of five microcystins were linear in the range of 5~100 μg/L with correlation coefficients more than 0.995, the recoveries of five compounds ranged from 76.0% to 118%, with RSDs(n=6) of 1.9%~12.0%. The limit of detection and quantitation were in the range of 2~3 and 8~12 μg/kg respectively. The method was successfully used to detect the sediment samples from West Taihu Lake.
Key words:  Microcystins  UPLC MS/MS  ASE  SPE  Sediment