| 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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| 引用本文： | 吴海燕,郭萌萌,邴晓菲,郑关超,彭吉星,谭志军,翟毓秀. 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[J]. 海洋与湖沼, 2017, 48(3): 508-515 |
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| 作者姓名： | 吴海燕 郭萌萌 邴晓菲 郑关超 彭吉星 谭志军 翟毓秀 |
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| 作者单位： | 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;国家水产品质量监督检验中心 青岛 266071,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;国家水产品质量监督检验中心 青岛 266071,上海海洋大学水产与生命学院 上海 201306,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;国家水产品质量监督检验中心 青岛 266071,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;国家水产品质量监督检验中心 青岛 266071,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;国家水产品质量监督检验中心 青岛 266071,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;国家水产品质量监督检验中心 青岛 266071 |
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| 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。 |
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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,dc STX)、脱氨甲酰基新石房蛤毒素(Decarbaoylneosaxitoxin,dc NEO)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12(Gonyautxins-1-2,GTX12)为12.0μg/kg,膝沟藻毒素34(Gonyautxins-3-4,GTX34)、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,dc GTX3)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,dc GTX2)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。
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| 关 键 词： | 麻痹性贝类毒素 基质效应 固相萃取 |
| 收稿时间： | 2016-10-26 |
| 修稿时间： | 2017-01-13 |
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-Yan,GUO Meng-Meng,BING Xiao-Fei,ZHENG Guan-Chao,PENG Ji-Xing,TAN Zhi-Jun and ZHAI Yu-Xiu. SIMULTANEOUS IDENTIFICATION AND DETECTION OF PARALYTIC SHELLFISH TOXIN IN BIVALVE MOLLUSKS BY LIQUID CHROMATOGRAPHY COUPLED WITH QUADRUPOLE/LINEAR ION TRAP TANDEM MASS SPECTROMETRY[J]. Oceanologia Et Limnologia Sinica, 2017, 48(3): 508-515 |
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| Authors: | WU Hai-Yan GUO Meng-Meng BING Xiao-Fei ZHENG Guan-Chao PENG Ji-Xing TAN Zhi-Jun ZHAI Yu-Xiu |
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| Affiliation: | 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;National Center for Quality Supervision and Test of Aquatic Products, Qingdao 266071, China,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;National Center for Quality Supervision and Test of Aquatic Products, Qingdao 266071, China,College of Fisheries and Life Science, Shanghai Ocean University, Shanghai 201306, China,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;National Center for Quality Supervision and Test of Aquatic Products, Qingdao 266071, China,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;National Center for Quality Supervision and Test of Aquatic Products, Qingdao 266071, China,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;National Center for Quality Supervision and Test of Aquatic Products, Qingdao 266071, China and 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;National Center for Quality Supervision and Test of Aquatic Products, Qingdao 266071, China |
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| Abstract: | |
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| Keywords: | paralytic shellfish toxins matrix suppression effect solid-phase extraction |
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