水产品及螺旋藻片中微囊藻毒素检测方法研究  

Determination of Microcystins in Aquatic Products and Spirulina Powder Ablets by Ultra Performance Liquid Chromatography -Tandem Mass Spectrometry

作　　者：雷云[1] 戴明 周鹏 郑小严 林钦 欧阳立群 

机构地区：[1]福建医科大学药学院药物分析系,福建福州350004 [2]福建省产品质量检验研究院国家加工食品质量监督检验中心,福建福州350002

出　　处：《食品研究与开发》2013年第13期87-91,共5页Food Research and Development

基　　金：福建省自然科学基金(2009J05115&2010J05019);福建省卫生厅基金(2010-1-34)

摘　　要：建立了超高效液相色谱-串联质谱法检测水产品及螺旋藻片中微囊藻毒素的高灵敏度色质联用快速检测方法。样品经溶剂超声提取、固相萃取净化,氮气吹至近干并定容后,通过超高效液相色谱-串联四极杆质谱仪检测。分离柱为Waters Acquity BEH C18柱(1.7μm,2.1 mm×100 mm);流动相为0.3%甲酸水溶液-乙腈;流速0.4 mL/min。4种不同基质样品中有害毒素微囊藻毒素MCYST-RR和MCYST-LR的检测限分别为0.7μg/kg和0.3μg/kg。4种不同基质样品中微囊藻毒素的回收率为80.0%～103.6%,相对标准偏差(RSD)为2.2%～14.6%(n=5),在0.01μg/mL～10μg/mL浓度范围内呈良好的线性关系,线性回归系数r2均大于0.999。A simple and rapid method was developed for the determination of microcystin-RR and microcystin- LR in aquatic product and spirulina powder ablets by ultra performance liquid chromatography tandem mass spectrometric （UHPLC-MS/MS）. The analytes were extracted from aquatic products and spirulina powder ablets using butanol：methanol：water （1 ： 4 ： 15,volume ratio）with ultrasonication, followed by a solid-phase extraction （SPE） on Oasis HLB and silica cartridges. After the chromatographic separation on Waters Aequity BEH C 18 （ 1.7um, 2.1 mmx 100 mm）column by 0.3 % formic aeid-acetonitrile isocratic elution, the analysis was carried out by UHPLC-MS/MS. The linear range of microcystins in aquatic products and spirulina powder ablets were 0.01 Ixg/mL-10 ug/mL （r2〉0.99） and the limits of detection were 0.7 p^g/kg for MCYST-RR and 0.3 ug/kg for MCYST-LR. The recoveries were ranged from 80.0 %-103.6 %, and the relative standard deviations were 2.2 %-14.6 %（n=5）.

关 键 词：超高效液相色谱-串联质谱法 水产品 螺旋藻片 微囊藻毒素 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程]