岳亚军,张律,曾丽兰.高效液相色谱-串联质谱法测定双壳类水产品麻痹性贝类毒素[J].中国食品卫生杂志,2017,29(5):571-576. 本文二维码信息
二维码(扫一下试试看!)
高效液相色谱-串联质谱法测定双壳类水产品麻痹性贝类毒素
Determination of paralytic shellfish poisoning in bivalves aquatic products by high performance liquid chromatography-mass spectrometry
投稿时间:2017-05-25  
DOI:
中文关键词:  双壳类  麻痹性贝类毒素  生物毒素  高效液相色谱-串联质谱  固相萃取  基质效应  检测  食品安全
Key Words:Bivalves  paralytic shellfish poisoning  biotoxin  high performance liquid chromatography-mass spectrometry  solid phase extraction  matrix effect  test  food safety
基金项目:
作者单位E-mail
岳亚军 深圳市罗湖区疾病预防控制中心,广东 深圳 518020 yueyajun1978@126.com 
张律 深圳市罗湖区疾病预防控制中心,广东 深圳 518020  
曾丽兰 深圳市罗湖区疾病预防控制中心,广东 深圳 518020  
摘要点击次数: 309
全文下载次数: 132
中文摘要:
      目的 采用Supelco ENVI-Carb柱净化双壳类水产品中的麻痹性贝类毒素(PSP),建立高效液相色谱-串联质谱(HPLC-MS/MS)法检测双壳类水产品中的PSP,为水产品中的PSP检测提供方法依据。方法 选用色谱柱TSK-GEL Amide-80(2.0 mm×250 mm,5 μm),以2 mmol/L甲酸铵-50 mmol/L甲酸水和95%乙腈水(含2 mmol/L甲酸铵-50 mmol/L甲酸)为流动相,采用梯度洗脱进行分离。样品用1%乙酸溶液进行提取,上清液加入氨水后(pH=4.0)经Supelco ENVI-Carb柱净化,将洗脱液抽干收集,上机测定。多重反应监测(MRM)模式检测。结果 PSP的线性范围为8.1~705.0 μg/kg,检出限为10~35 μg/kg,回收率在47.0%~91.3%之间。结论 本方法提取效果好、基质效应小,适用于双壳类水产品中麻痹性贝类毒素的痕量检测。
Abstract:
      Objective To extract paralytic shellfish poisoning (PSP) with Supelco ENVI-Carb cartridge, develop a high performance liquid chromatography-mass spectrometry (HPLC-MS/MS) method for determination of PSP in bivalves aquatic products, and provide proof for the detection of PSP in aquatic products. Methods PSP was extracted by 1% acetic acid solution, supernatant added with ammonia (pH=4.0) was loaded on Supelco ENVI-Carb cartridge, and the eluent was dried up. Then the sample was separated on a TSK-GEL Amide column (2.0 mm×250 mm, 5 μm) with water contained 2 mmol/L ammonium formate-50 mmol/L formic acid and 95% acetonitrile contained 2 mmol/L ammonium formate-50 mmol/L formic acid was mobile phase for gradient elution. Detection was carried out by multiple reaction monitoring. Results PSP had a good linear result in the range of 8.1-705.0 μg/kg with detection limit of 10-35 μg/kg in bivalves aquatic products. The recovery was 47.0%-91.3%. Conclusion This method had good performance of extraction and with low matrix inhibition effect. The assay was suitable for trace detection of paralytic shellfish poisoning in bivalves aquatic products.
查看全文  查看/发表评论  下载PDF阅读器