摘要
目的建立织纹螺组织中3种腹泻性贝类毒素（diarrhetic shellfish toxins,DSTs）：大田软海绵酸（okadaic acid,OA）;鳍藻毒素-1（dinophysistoxin-1,DTX-1）;鳍藻毒素-2（dinophysistoxin-2,DTX-2）的超高效液相色谱-串联质谱（UPLC-MS/MS）检测方法。方法样本经甲醇∶水（4∶1,V/V）溶液提取,经正己烷脱脂和C18固相萃取柱净化,经ACQUITY UPLC BEH C18（1.7μm,2.1mm×100mm）色谱柱分离,乙腈-甲酸溶液（10 mmoL/L）为流动相,流速为0.2 ml/min,柱温为30℃,负离子扫描,在多反应监测（MRM）模式下进行定性与定量分析。结果 OA、DTX-1、DTX-2在（0.01-0.20）mg/L范围内线性关系良好,3个添加水平的平均回收率为80.3%-93.6%,相对标准偏差（RSD）为2.13%-4.23%。其定量限（LOQ）为6.93μg/kg、3.3μg/kg、4.95μg/kg。结论利用此方法发现福建织纹螺中含有腹泻性贝类毒素,方法灵敏度高,操作简便,适用于实际样本的分析检测。
Objective To determine three diarrheic shellfish toxins（DSTs）by using ultra performance liquid chromatography-mass/mass spectrometry（UPLC-MS/MS）in Nassariidae. Methods Nassariidae samples were collected and extracted by methanol and water（4∶1,V/V）.Nassariidae extraction solution was processed with n-hexane and then purified by C18solid-phase extraction column.The three DSTs including Okadaic acid（OA）,Dinophysistoxin-1（DTX-1）and Dinophysistoxin-2（DTX-2）were separated on a reversed phase ACQUITY UPLC BEH C18（1.7μm,2.1mm×100mm）column using acetonitrile-10mmoL/L formic acid in water as mobile phase,with a flow rate at 0.2ml/min and a column temperature of 30℃and then were qualified and quantified by ultra performance liquid chromatography-mass/mass spectrometry under multiple reaction monitoring（MRM）. Results The method showed a good linearity of three DSTs in the range of0.01-0.2mg/L.The average recoveries ranged from 80.3%to 93.6%at three spiked concentrations with the relative standard deviation of 2.13%to 4.23%.The quantification limits（LOQ）（S/N≥10）of the method for three DSTs were 6.93μg/kg,3.3μg/kg and 4.95μg/kg,respectively. Conclusions By the established method,DSTs are detected in Nassariidae in Fujian,the method is highly sensitive and simple,and is suitable for determination of DST in many kinds of samples.
出处
《中国预防医学杂志》
CAS
2016年第6期414-418,共5页
Chinese Preventive Medicine
基金
福建省自然科学基金资助项目(2015J01296)
福建省卫生计生委青年科研课题资助项目[2014-01-27]
关键词
超高效液相色谱-串联质谱法
织纹螺
腹泻性贝类毒素
固相萃取
Ultra performance liquid chromatography-mass/mass spectrometry
Nassariidae
Diarrhetic shellfish toxin
Solid-phase extraction
