摘要
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.
作者
徐潇颖
刘柱
毛思浩
陈晶燕
张文萍
梁晶晶
XU Xiaoying;LIU Zhu;MAO Sihao;CHEN Jingyan;ZHANG Wenping;LIANG Jingjing(Zhejiang Institute for Food and Drug Control,Hangzhou 310052,China)
出处
《食品科技》
CAS
北大核心
2023年第4期305-311,共7页
Food Science and Technology
基金
浙江省公益技术研究计划(分析测试)项目(LGC21C200001)
浙江省市场监督管理局检验监测技术装备项目(ZB2022466)。