全自动在线固相萃取-高效液相色谱-串联质谱法测定螺旋藻中8种微囊藻毒素

Simultaneous Determination of Eight Microcystins in Spirulina by High Performance Liquid Chromatography-Tandem Mass Spectrometry with Automatic Solid Phase Extraction

通过全自动固相萃取(Auto-SPE)-高效液相色谱-串联质谱法(HPLC-MS/MS)实现了螺旋藻中8种微囊藻毒素(MCs)的同时测定。螺旋藻样品经80%(体积分数)的乙腈-水溶液超声提取,选用C_(18)固相萃取小柱进行全自动在线净化后,采用电喷雾正离子多反应模式监测进行分析。通过外标法定量,8种MCs在2~50μg/kg范围内线性关系良好(相关系数R^(2)不小于0.99),检出限均为0.5μg/kg,定量限2.0μg/kg。在阴性螺旋藻样品3个不同浓度的加标实验中,回收率在76.5%~99.6%之间,相对标准偏差在1.1%~4.7%之间。该方法低成本、重现性好、灵敏度高,适用于螺旋藻中多种MCs的定量测定。

Simultaneous determination of eight microcystins(MCs)in Spirulina platensis was achieved by automatic solid phase extraction(auto SPE)-high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS).The sample was ultrasound extracted by 80%(v/v)acetonitrile.The liquid substances were purified by C_(18) column with automatic solid phase extraction(auto-SPE)and analyzed by ESI-MS/MS in the positive ion scan MRM mode.The external standard method was used for the quantification.The linear ranges for 8 MCs were 2~50μg/kg,and the correlation coefficients were not less than 0.99.The limits of detection were 0.5μg/kg.The limits of quantification were 2.0μg/kg.The recoveries of the 8 MCs spiked in blank Spirulina samples ranged from 76.5% to 99.6%with the relative standard deviations of 1.1%~4.7%.The method has the advantages of low cost,good reproducibility and high sensitivity.It is suitable for the quantitative determination of multiple MCs in Spirulina.