分析测试学报2025，Vol.44Issue(10)：2169-2176,8.DOI:10.12452/j.fxcsxb.241129561
QuEChERS/超高效液相色谱-串联质谱法同时测定水产品中8种微囊藻毒素和2种腹泻性贝类毒素
Simultaneous Determination of 8 Microcystins and 2 Diarrhoeal Shellfish Poisons in Aquatic Products by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry Based on QuEChERS Purification
摘要
Abstract
A reliable method was developed for the simultaneous determination of 8 microcystins and 2 diarrhoeal shellfish toxins in aquatic products by QuEChERS purification combined with ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS).The Crucian carp and Litopenaeus vannamei samples were extracted with 95%methanol and purified by anhydrous Mg-SO4,graphitized carbon black(GCB)and octadecylsilane bonded silica gel(C18).The filtrate was an-alyzed by a Waters ACQUITY UPLC® HSS T3 chromatographic column(2.1 mm×150 mm,1.8 μm)with mobile phase consisting of 0.1%formic acid and 5 mmol/L ammonium formate and methanol.10 algal toxins were qualitatively and quantitatively analyzed by positive and negative electrospray ioniza-tion modes,detected by multiple reaction monitoring(MRM)mode and quantified by external stan-dard method.The results showed that 10 algal toxins in Crucian carp and Litopenaeus vannamei showed good linear correlations with correlation coefficients(r2)not less than 0.999 0 in the corre-sponding concentration ranges,and the limits of detection(LODs)and limits of quantitation(LOQs)were in the ranges of 0.1-5.0 μg/kg and 0.5-10 μg/kg,respectively.Average recoveries of the 10 algal toxins in Crucian carp and Litopenaeus vannamei at three different spiked levels were 79.5%-120%and 73.2%-103%,and the relative standard deviations(RSDs,n=6)were 1.2%-14%and 1.1%-16%,respectively.The established method was applied to the analysis of 23 samples of Crucian carp,2 Silver carp and 30 Litopenaeus vannamei samples in Shanghai,and MC-LR,MC-RR and MC-LF as the mainly detected algin toxins.This method is simple,rapid,effective,highly sensitive,and is suitable for the qualitative identification and content determination of 10 algal toxins in aquatic products.关键词
QuEChERS/超高效液相色谱-串联质谱法/微囊藻毒素/腹泻性贝类毒素/水产品Key words
QuEChERS/ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)/microcystins(MCs)/diarrhetic shellfish poison(DSP)/aquatic products分类
化学化工引用本文复制引用
刘晓瑾,黄晴雯,郭大凯,王欣艺,陆思言,聂冬霞,韩铮..QuEChERS/超高效液相色谱-串联质谱法同时测定水产品中8种微囊藻毒素和2种腹泻性贝类毒素[J].分析测试学报,2025,44(10):2169-2176,8.基金项目
绿色食品(绿色优质农产品)高质量创新发展技术研究项目(GFJY2024007) （绿色优质农产品）
上海市农业科学院科研课题项目(农科应基2024(09)) （农科应基2024(09）
