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
钟润生,博士,副教授,研究方向:颗粒物与污染物相互作用及其环境行为,E-mail:runsoon@qq.com
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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.
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。
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.
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
ultrahigh performance liquid chromatography-tandem mass spectrometrysolid phase extractionphycotoxinsseawatersuspended particulate mattersediment
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