同位素稀释-液相色谱-串联质谱法测定4类水产品中甲霜灵的残留量  

Determination of Metalaxyl Residue in 4 Aquatic Products by Isotope Dilution-Liquid Chromatography-Tandem Mass Spectrometry

作　　者：张俊 黄冬梅[2] 黄宣运[2] 史永富[2] 王媛[2] 田良良[2] ZHANG Jun;HUANG Dongmei;HUANG Xuanyun;SHI Yongfu;WANG Yuan;TIAN Liangliang(College of Food Science&Technology,Shanghai Ocean University,Shanghai 201306,China;Key Laboratory of Control of Quality and Safety for Aquatic Products(Shanghai)of the Ministry of Agriculture and Rural Affairs,East China Sea Fishery Research Institute,Chinese Academyof Fishery Sciences,Shanghai 200090,China)

机构地区：[1]上海海洋大学食品学院,上海201306 [2]中国水产科学研究院东海水产研究所,农业农村部水产品质量安全控制重点实验室(上海),上海200090

出　　处：《理化检验（化学分册）》2024年第3期249-254,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：农业农村部农业标准制修订项目(农质标函[2019]77号)资助。

摘　　要：提出了同位素稀释-液相色谱-串联质谱法测定鱼、虾、蟹、贝4类水产品中甲霜灵残留量的方法。取样品(5±0.05)g,加入10 ng的内标甲霜灵-d 6,静置10 min,用10 mL含1%(体积分数)乙酸的乙腈溶液涡旋混合、离心。取上清液,于45℃氮吹至0.5 mL以下,加入7.5 mL 20%(体积分数,下同)乙腈溶液混匀,用7.5 mL正己烷去脂,Agela Cleanert S C_(18)固相萃取柱富集净化。所得溶液于45℃氮吹至干,用1 mL 20%乙腈溶液复溶,混匀后过0.22μm针式水相尼龙滤膜,滤液收集至进样小瓶中。以SHISEIDO CAPCELL PAK C_(18)色谱柱为固定相,以不同体积比的0.1%(体积分数)甲酸溶液和乙腈的混合液为流动相进行梯度洗脱,内标法定量。结果表明,甲霜灵标准曲线的线性范围为1.0~100.0μg·L^(-1),检出限(3S/N)为0.5μg·kg^(-1)。以不同品种水产品为空白基质,在1.0,2.0,10.0μg·kg^(-1)等3个浓度水平下,甲霜灵的回收率为93.8%~105%,测定值的相对标准偏差(n=6)均小于13%。A method was proposed for the determination of metalaxyl residues in 4 aquatic products(fish,shrimp,crab and shellfish)by isotope dilution-liquid chromatography-tandem mass spectrometry.The sample(5±0.05)g was taken,and 10 ng of internal standard metalaxyl-d 6 was added,settling for 10 min.Then the mixture was vortex mixed and centrifuged in 10 mL of acetonitrile solution containing 1%(volume fraction)acetic acid.The supernatant was blown to less than 0.5 mL by nitrogen at 45℃,and then 7.5 mL of 20%(volume fraction,the same below)acetonitrile solution was added to mix well.7.5 mL of n-hexane was used to defat,and Agela Cleanert S C_(18)solid phase extraction column was used for enrichment and purification.The obtained solution was blown to dryness by nitrogen at 45℃,and the residue was redissolved in 1 mL of 20%acetonitrile solution.After mixed well,the solution was passed through 0.22μm needle aqueous nylon filter membrane and the filtrate was collected into the sample vial.SHISEIDO CAPCELL PAK C_(18)column was used as stationary phase,and gradient elution was performed with a mixture of 0.1%(volume fraction)formic acid solution and acetonitrile at different volume ratios as mobile phase.The internal standard method was used for quantitative analysis.As shown by the results,linear range of the standard curve of metalaxyl was 1.0-100.0μg·L^(-1),with detection limit(3S/N)of 0.5μg·kg^(-1).Using different varieties of aquatic products as blank matrices,the recovery ranged from 93.8%to 105%at 3 concentration levels of 1.0,2.0,10.0μg·kg^(-1),with RSDs(n=6)of the determined values less than 13%.

关 键 词：甲霜灵 水产品 同位素稀释法 液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学]