高效液相色谱-串联质谱法测定水产品中3种微囊藻毒素含量  

Determination of Microcystin-LR,Microcystin-RR and Microcystin-YR in Aquatic Products by means of HPLC-MS-MS

作　　者：梁振纲 徐志伟[2] 陈艺玮[2] 邓世明[1] 徐莉[2] 

机构地区：[1]海南大学海洋学院,海南海口570228 [2]海南出入境检验检疫局技术中心,海南海口570311

出　　处：《江西农业大学学报》2015年第6期1069-1075,共7页Acta Agriculturae Universitatis Jiangxiensis

基　　金：海南省科技兴海专项资金项目(XH201407;XH201309)

摘　　要：建立高效液相色谱-串联质谱法测定水产品中microcystin-LR、microcystin-RR、microcystin-YR 3种微囊藻毒素含量的方法,对方法的提取、净化条件和微囊藻毒素可能的质谱裂解机理进行研究。采用甲醇提取,HLB固相萃取柱净化,液相色谱-质谱/质谱进行检测,外标法定量,测定低限为5μg/kg,以鱼、虾、牡蛎为阴性样品,添加水平为0.005 mg/kg、0.010 mg/kg、0.020 mg/kg时,回收率范围为85.2%～94.3%,相对标准偏差为4.7%～8.1%。经验证,此方法灵敏度、特异性和选择性均能满足水产品中微囊藻毒素的检测要求。A HPLC-MS-MS method was developed for determining microcystin-LR,microcystin-RR and microcystin-YR in seafoods,the conditions of extraction,purification and the pyrolysis mechanism were also discussed.Methanol was used as the extraction solvent and HLB solid phase extraction column was used as the purifier.External standard method was used to quantify the target compounds with LC-MS-MS.The tested matrix included fish,prawn,oysters.The limits of detection were 5μg / kg.3 spiked levels（ 0.005 mg / kg,0.010 mg / kg and 0.020 mg / kg） were applied,and the average recoveries and RSDs obtained were ranged from 85. 2% ～99.3% and 4.7% ～ 8.1%,respectively.As proved,this method satisfies the requirements（ including sensitivity,specificity and selectivity） for determining microcystin-LR,microcystin-RR,microcystin-YR.

关 键 词：微囊藻毒素 高效液相色谱-串联质谱 水产品 

分 类 号：Q936[生物学—微生物学]