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

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