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,5μm),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8.1~705.0μg/kg,检出限为10~35μg/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。 Objective To determine PSP in bivalve aquatic products by HPLC using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) with Supelco ENVI-Carb column to purify PSP from shellfish, PSP detection for aquatic products provide a method basis. Methods The chromatographic column TSK-GEL Amide-80 (2.0 mm × 250 mm, 5 μm) was used. The column was eluted with 2 mmol / L ammonium formate-50 mmol / L formic acid and 95% acetonitrile in water / L formic acid) as mobile phase, using gradient elution to separate. The samples were extracted with 1% acetic acid solution. The supernatant was purified by Supelco ENVI-Carb column after addition of aqueous ammonia (pH = 4.0). The eluate was collected by suction and centrifuged. Multiple Reaction Monitoring (MRM) Pattern Detection. Results The linear range of PSP was 8.1 ~ 705.0μg / kg with the detection limit of 10 ~ 35μg / kg and the recovery of 47.0% ~ 91.3%. Conclusion The method has good extraction effect and small matrix effect and is suitable for the trace detection of paralytic shellfish toxins in bivalve aquatic products.