Determination of Residue of Emamectin in Aquatic Products by Liquid Chromatography Tandem Mass Spectrometry
摘 要
提出了液相色谱-串联质谱法(LC-MS/MS)测定水产品中甲氨基阿维菌素残留量的方法。取水产样品5.00 g,用12.5 mL乙酸乙酯超声10 min,振荡15 min,重复提取一次,合并上清液并用乙酸乙酯定容至25 mL。取0.5 mL上述溶液,于45℃氮吹至干,残渣用80%(体积分数)乙腈溶液1 mL溶解,超声后用乙腈饱和正己烷溶液2 mL液液萃取净化。净化后的下层溶液过0.22 μm疏水性聚四氟乙烯(PTFE)滤膜,在Atlantis T3色谱柱上分离,以不同体积比的乙腈和5 mmol·L-1甲酸溶液混合液为流动相进行梯度洗脱,用LC-MS/MS检测,外标法定量。结果表明,甲氨基阿维菌素的质量浓度在0.01~2.0 μg·L-1内与对应的峰面积呈线性关系,测定下限(10S/N)为0.5 μg·kg-1。按照标准加入法进行回收试验,回收率为84.3%~99.9%,测定值的相对标准偏差(n=6)均小于7.0%。方法用于分析50个实际样品,仅1个进口鲑鱼检出甲氨基阿维菌素,检出量为20.7 μg·kg-1。
Abstract
A method was proposed for the determination of residue of emamectin in aquatic products by liquid chromatography tandem mass spectrometry (LC-MS/MS). 5.00 g of aquatic product sample was taken and ultrasonically extracted for 10 min with 12.5 mL of ethyl acetate, and then shaken by oscillation for 15 min. The extraction was repeated once, and the combined supernatant was made its volume up to 25 mL with ethyl acetate. 0.5 mL of the above solution was taken and blown to dryness by nitrogen at 45℃, then the residue was dissolved in 1 mL of 80% (volume fraction) acetonitrile solution. After ultrasound, the above solution was purified by liquid-liquid extraction with 2 mL of acetonitrile saturated n-hexane solution. After purification, the lower layer solution was passed through 0.22 μm hydrophobic polytetrafluoroethylene (PTFE) filter membrane, and separated on Atlantis T3 column using a mixture of acetonitrile and 5 mmol·L-1 acetic acid solution at different volume ratios for gradient elution, and determined by LC-MS/MS, with external standard method for quantitation. As shown by the results, linear relationship between the mass concentration of emamectin and the corresponding peak area was found in the range of 0.01-2.0 μg·L-1, with the lower limit of determination (10S/N) of 0.5 μg·kg-1. Test for recovery was made by the standard addition method, giving the results in the range of 84.3%-99.9%, with RSDs (n=6) of the determined values less than 7.0%. This method was applied to analysis of 50 actual samples, and emamectin was detected in only one imported salmon sample, with detection amount of 20.7 μg·kg-1.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202312006
所属栏目 工作简报
基金项目 国家十四五重点研发项目子课题(2022YFF1100804)
收稿日期 2022/9/30
修改稿日期
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联系人作者欧阳少伦(oyshl@163.com)
备注蓝草,工程师,硕士,研究方向为兽药残留检测
引用该论文: LAN Cao,OUYANG Shaolun,ZOU You,SHAO Linzhi. Determination of Residue of Emamectin in Aquatic Products by Liquid Chromatography Tandem Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2023, 59(12): 1401~1406
蓝草,欧阳少伦,邹游,邵琳智. 液相色谱-串联质谱法测定水产品中甲氨基阿维菌素的残留量[J]. 理化检验-化学分册, 2023, 59(12): 1401~1406
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【6】LOVE D C, FRY J P, CABELLO F, et al. Veterinary drug use in United States net pen salmon aquaculture:Implications for drug use policy[J]. Aquaculture, 2020,518:734820.
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【11】易锡斌,梁玉树,黄晓琴,等.UPLC-MS/MS同时测定蔬菜中阿维菌素等5种常用农药残留量[J].分析测试学报, 2015,34(7):829-835.
【12】罗莉,吴生文,林培,等.使用液质联用对特香型白酒酿造原料大米中农药残留检测的研究[J].酿酒, 2020,47(4):84-89.
【13】何红梅,赵华,张春荣,等.超高效液相色谱-串联质谱法测定粮谷中阿维菌素类杀虫剂残留[J].分析化学, 2013,41(11):1627-1632.
【14】寿林飞,张文童,虞淼,等.液相色谱-串联质谱法测定植物油中阿维菌素和甲维盐残留[J].浙江农业科学, 2013,54(12):1651-1653.
【15】UCLÉS S, LOZANO A, SOSA A, et al. Matrix interference evaluation employing GC and LC coupled to triple quadrupole tandem mass spectrometry[J]. Talanta, 2017,174:72-81.
【16】KRUVE A, KVNNAPAS A, HERODES K, et al. Matrix effects in pesticide multi-residue analysis by liquid chromatography-mass spectrometry[J]. Journal of Chromatography A, 2008,1187(1/2):58-66.
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