Determination of 18 Phycotoxins in Seawater，Suspended Particulate Matter and Sediment by Ultrahigh Performance Liquid Chromatography－Tandem Mass Spectrometry

LI Jing; YAN Meng; SHEN Jin-can; XIAO Chen-gui; MAK Yim-ling; LI Yang; GUO Jian-ning; ZHONG Run-sheng

doi:10.19969/j.fxcsxb.22081704

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Determination of 18 Phycotoxins in Seawater，Suspended Particulate Matter and Sediment by Ultrahigh Performance Liquid Chromatography－Tandem Mass Spectrometry

Scientific Papers | 更新时间：2023-02-28

- Determination of 18 Phycotoxins in Seawater，Suspended Particulate Matter and Sediment by Ultrahigh Performance Liquid Chromatography－Tandem Mass Spectrometry
- Journal of Instrumental Analysis Vol. 42, Issue 2, Pages: 181-188(2023)
- 作者机构：
  
  1.深圳信息职业技术学院交通与环境学院，广东深圳 518172
  2.香港城市大学海洋污染国家重点实验室，香港 999077
  3.深圳海关食品检验检疫技术中心深圳市食品安全检测技术研发重点实验室，广东深圳 518026
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.22081704
  CLC：
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李静,晏萌,沈金灿等.UPLC－MS/MS测定海水、悬浮颗粒物及沉积物中18种藻毒素[J].分析测试学报,2023,42(02):181-188.

LI Jing,YAN Meng,SHEN Jin-can,et al.Determination of 18 Phycotoxins in Seawater，Suspended Particulate Matter and Sediment by Ultrahigh Performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(02):181-188.
李静,晏萌,沈金灿等.UPLC－MS/MS测定海水、悬浮颗粒物及沉积物中18种藻毒素[J].分析测试学报,2023,42(02):181-188. DOI： 10.19969/j.fxcsxb.22081704.

LI Jing,YAN Meng,SHEN Jin-can,et al.Determination of 18 Phycotoxins in Seawater，Suspended Particulate Matter and Sediment by Ultrahigh Performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(02):181-188. DOI： 10.19969/j.fxcsxb.22081704.

摘要

采用固相萃取结合超高效液相色谱－串联质谱（UPLC－MS/MS）同时检测18种海洋藻毒素，包括原多甲藻酸贝类毒素（AZAs）、裸藻毒素（BTXs）、太平洋雪卡毒素（P－CTXs）、鳍藻毒素（DTXs）、米氏裸甲藻贝类毒素（GYM）、刺尾鱼素（MTX3）、大田软骨酸毒素（OA）、扇贝毒素（PTX2）、螺环内酯毒素（SPX1）及虾夷扇贝毒素（YTXs）。海水（1 L）或悬浮颗粒物及沉积物（1 g）的超声萃取液经Agilent Bond Elut C,18,（500 mg/6 mL）固相萃取柱净化萃取后，在洗脱液中加入10%丙三醇－甲醇溶液以减少目标物损失。以95%乙腈水和水（两相均含有0.1%甲酸和2 mmol/L甲酸铵）为流动相，目标物经Phenomenex Kinetex C,18,色谱柱（100 mm × 2.1 mm i.d.，1.7 μm）分离，采用电喷雾串联质谱多反应监测模式下正、负离子同时检测，外标法定量。18种藻毒素在6 min内分离良好，在线性范围内的相关系数为0.991 1 ~ 0.999 9，定量下限为0.05 ~ 250 pg/L（或pg/g）。三水平六平行的加标回收率为77.4% ~ 119%，相对标准偏差为1.1% ~ 15%。采用该方法在深圳珠江口28个采样点的海水样品中共检出10种藻毒素，其中PTX2（36.6 ~ 7 900 pg/L）为最主要检出藻毒素，MTX3（0 ~ 262 pg/L）在我国海域中首次检出。该方法具有良好的灵敏度和精密度，满足实际海水、悬浮颗粒物及沉积物样品中藻毒素的同时检测要求。

Abstract

A method was established for the simultaneous detection of 18 marine phycotoxins by ultrahigh performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS） combined with solid phase extraction，including azaspiracids（AZAs），brevetoxins（BTXs），Pacific ciguatoxins（P－CTXs），dinophysistoxins（DTXs），gymnodimine（GYM），maitotoxin3（MTX3），okadaic acid（OA），pectenotoxin2（PTX2），spirolide1（SPX1） and yessotoxins（YTXs） etc．Seawater（1 L） or the ultrasonic extracts of suspended particulate matter or sediment（1 g） was extracted with solid phase extraction cartridges（Agilent Bond Elut C,18,，500 mg/6 mL），and then 10% glycerol－methanol was added to the eluent to reduce the loss of target toxins．Water was the aqueous phase and 95% acetonitrile/water was the organic phase，both of which contained 0.1% formic acid and 2 mmol/L ammonium formate．A Phenomenex Kinetex C,18, column（100 mm × 2.1 mm i.d.，1.7 μm） was used to separate the phycotoxins in six minutes，and then the target analytes were detected by UPLC－MS/MS in multiple reaction monitoring mode．The external standard method was used for the quantitation of 18 phycotoxins．The correlation coefficients of standard curves were 0.991 1－0.999 9．The quantitation limits of the methed for 18 phycotoxins ranged from 0.05 to 250 pg/L（or pg/g）．The matrix-spiked recoveries for 18 phycotoxins ranged from 77.4% to 119%，with the relative standard deviations of 1.1%－15%．Ten phycotoxins were detected in seawater from the Pearl River Estuary，with the predominant PTX2 of 36.6－7 900 pg/L．MTX3 concentrations ranging from 0 to 262 pg/L was monitored for the first time．With good sensitivity and precision，this method can satisfy the requirements for simultaneous determination of 18 phycotoxins in seawater，suspended particulate matter and sediment.

关键词

超高效液相色谱－串联质谱固相萃取藻毒素海水悬浮颗粒物沉积物

Keywords

ultrahigh performance liquid chromatography－tandem mass spectrometrysolid phase extractionphycotoxinsseawatersuspended particulate mattersediment

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