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| 液相色谱-四极杆/线性离子阱复合质谱测定双壳贝类中麻痹性贝类毒素 |
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吴海燕1,2, 郭萌萌1,2, 邴晓菲3, 郑关超1,2, 彭吉星1,2, 谭志军1,2, 翟毓秀1,2
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1.农业部水产品质量安全检测与评价重点实验室 中国水产科学研究院黄海水产研究所 青岛 266071;2.国家水产品质量监督检验中心 青岛 266071;3.上海海洋大学水产与生命学院 上海 201306
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| 摘要: |
| 采用液相色谱-四极杆/线性离子阱复合质谱，建立了双壳贝类中13种麻痹性贝类毒素的定性确证和定量分析方法。样品经乙酸水溶液提取，石墨化碳黑固相萃取净化，亲水性液相色谱柱（hydrophilic interaction liquid chromatography，HILIC）分离；质谱采集使用独有的多反应监测-信息依赖性采集-增强子离子扫描模式。13种目标物线性范围相关系数不低于0.99，检出限为62.0μg STX eq/kg，其中石房蛤毒素（Saxitoxin，STX）、新石房蛤毒素（Neosaxitoxin，NEO）、脱氨甲酰基石房蛤毒素（Decarbamoylsaxitoxin，dcSTX）、脱氨甲酰基新石房蛤毒素（Decarbaoylneosaxitoxin，dcNEO）以及N-磺酰氨甲酰基类毒素5（Gonyautoxin-5，GTX5）为10.0μg/kg，膝沟藻毒素1&2（Gonyautxins-1&-2，GTX1&2）为12.0μg/kg，膝沟藻毒素3&4（Gonyautxins-3&-4，GTX3&4）、N-磺酰氨甲酰基类毒素2（N-Sulfocarbamoylgonyautoxin-2，C2）和脱氨甲酰基膝沟藻毒素3（Decarbamoylgonyautoxins-3，dcGTX3）为4μg/kg，N-磺酰氨甲酰基类毒素1（N-Sulfocarbamoylgonyautoxin-1，C1）和脱氨甲酰基膝沟藻毒2（Decarbamoylgonyautoxins-2，dcGTX2）为13μg/kg。基质加标平均回收率为（79.6±10.4）%-（98.8±6.54）%。该方法能够有效降低贝类基质抑制效应，简化前处理过程并通过减少样品稀释倍数来显著提高方法灵敏度，使同分异构体达到基线分离，适用于双壳贝类中麻痹性贝类毒素的监控分析。 |
| 关键词: 麻痹性贝类毒素 基质效应 固相萃取 |
| DOI：10.11693/hyhz20161000229 |
| 分类号:O657.6 |
| 基金项目:中央级基本科研业务费专项资金资助项目，20603022015017-1号，20603022011004号；山东省重点研究计划，2016GSF120018号。 |
附件 |
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| SIMULTANEOUS IDENTIFICATION AND DETECTION OF PARALYTIC SHELLFISH TOXIN IN BIVALVE MOLLUSKS BY LIQUID CHROMATOGRAPHY COUPLED WITH QUADRUPOLE/LINEAR ION TRAP TANDEM MASS SPECTROMETRY |
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WU Hai-Yan1,2, GUO Meng-Meng1,2, BING Xiao-Fei3, ZHENG Guan-Chao1,2, PENG Ji-Xing1,2, TAN Zhi-Jun1,2, ZHAI Yu-Xiu1,2
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1.Key Laboratory of Testing and Evaluation for Aquatic Product Safety and Quality, Ministry of Agriculture, Yellow Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Qingdao 266071, China;2.National Center for Quality Supervision and Test of Aquatic Products, Qingdao 266071, China;3.College of Fisheries and Life Science, Shanghai Ocean University, Shanghai 201306, China
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| Abstract: |
| We developed a new method for simultaneous identification and detection of 13 paralytic shellfish toxins (PSTs) in bivalve mollusks using liquid chromatography coupled with quadrupole/linear ion trap tandem mass spectrometry (LC-QTrap/MS). Samples were extracted with acetic acid aqueous solution, and cleaned up in ENVI-Carb solid-phase extraction column. Separation of the 13 PSTs were performed on an HILIC (hydrophilic interaction liquid chromatography) with multiple reaction monitoring (MRM)-information-dependent acquisition (IDA) experiment-enhanced product ion (EPI) scan in mass spectrometry acquisition. The calibration curves are linear well with correlation coefficient over 0.99. The overall detection limit of the method is 62.0μg for STX eq/kg; specifically, the limit for STX, dcSTX, NEO, dcNEO, and GTX5 was 10.0μg/kg; 12.0μg/kg for GTX1; 4μg/kg for GTX3, GTX4, C2 and dcGTX3, and 13μg/kg for C1 and dcGTX2. The average spiked recoveries for 13PSTs were (79.6±10.4)%-(98.8±6.54)%. This method could reduce shellfish matrix suppression effect, simplify pre-treatment, reduce the times of dilution, and increase the sensitivity, during which isomers could be separated from baseline. The proposed method therefore is recommended to identify and detect the 13PSTs in bivalve mollusks. |
| Key words: paralytic shellfish toxins matrix suppression effect solid-phase extraction |