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超高效液相色谱-串联质谱法测定4种麻痹性贝类毒素
引用本文:张小军,陈雪昌,郭远明,梅光明,龙举,薛彬,郑斌.超高效液相色谱-串联质谱法测定4种麻痹性贝类毒素[J].浙江水产学院学报,2011(2):95-98.
作者姓名:张小军  陈雪昌  郭远明  梅光明  龙举  薛彬  郑斌
作者单位:[1]浙江海洋学院海洋与渔业研究所,浙江省海洋水产研究所,浙江省海水增养殖重点实验室,浙江舟山316100 [2]浙江省海洋开发研究院,浙江舟山316000
摘    要:建立了超高效液相色谱-串联四极杆质谱法测定贝类中4种麻痹性贝类毒素的方法。样品均质后经乙酸水溶液提取,HLB固相萃取柱净化,超高效液相色谱分离,串联四级杆质谱检测,外标法定量。STX、dcSTX、neoSTX、dcneoSTX在10.0~50.0μg/kg的添加范围内的平均回收率为77.4%~90.8%,相对标准偏差为3.87%~6.37%,定量检出限均为10.0μg/kg。该方法分析速度快、灵敏度高、重现性好,可广泛适用于贝类中麻痹性贝类毒素的测定。

关 键 词:超高效液相色谱-串联质谱法  麻痹性贝类毒素  测定

Determination of Four Paralytic Shellfish Poisons by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry
Institution:ZHANG Xiao-jun,CHEN Xue-chang,GUO Yuan-ming,et al(Marine and Fishery Research Institute of Zhejiang Ocean University,Zhejiang Marine Fisheries Research Institute,Zhejiang Province Key Lab of Mariculture & Enhancement,Zhoushan 316100,China)
Abstract:An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method was developed to determine four paralytic shellfish poisons(PSP).The sample,were extracted by HAC,then purified by SPE.Chromatographic separation was achieved by using UPLC,the detection was performed by tandem mass spectrometry.Results showed that the recoveries for STX,dcSTX,neoSTX,dcneoSTX at the addition of 10-50.0 μg/kg were ranged from 77.4% to 90.8% and the relative standard deviation was 3.87%-6.37%.The limit of quantity of the method was 10.0 μg/kg.The method is rapid and sensitive,suitable for determining of the PSP in shellfish.
Keywords:UPLC-MS/MS  paralytic shellfish poison  determination
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