首页|超高效液相色谱-串联质谱法测定水体和底泥中的阿维菌素和伊维菌素

超高效液相色谱-串联质谱法测定水体和底泥中的阿维菌素和伊维菌素

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为建立超高效液相色谱-串联质谱法(UHPLC-MS/MS)同时测定水产养殖环境(水体及底泥)中阿维菌素和伊维菌素的检测方法.先采用 HLB 固相萃取柱富集和净化水样,采用PSA和C18吸附剂净化底泥样品;样品中的目标物采用Phenomenex Kinetex C18色谱柱分离,以5 mmol/L乙酸铵水溶液和乙腈作为流动相进行梯度洗脱,在电喷雾离子源(ESI)、正离子扫描和多反应监测(MRM)模式下进行测定,外标法定量.在最优实验条件下,阿维菌素和伊维菌素在 7.5 min内完成色谱分离分析,目标物在 1~100 μg·L-1范围内线性关系良好,相关系数均大于 0.995.空白水样在 0.05,0.50,2.5 和5.0 μg·L-1共4 个添加水平下的回收率为71.6%~88.2%,相对标准偏差(RSD,n=6)在1.51%~8.81%,方法检出限(LOD)为 0.02 μg·L-1,方法定量限(LOQ)为0.05 μg·L-1;空白底泥在1.0,10.0,50.0 和100.0 ng·g-1共 4 个添加水平下的回收率为 75.3%~96.4%,RSD值(n=6)为 3.45%~8.99%,LOD值为 0.3 ng·g-1,LOQ值为 1.0 ng·g-1.该方法灵敏度高,重现性好,操作快速简便,适用于水产养殖环境(水体和底泥)中阿维菌素和伊维菌素的分析检测.
Determination of Avermectin and Ivermectin in Water and Sediment Using Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry
For the determination of avermectin and ivermectin in water and sediment from the aquaculture en-vironment,an ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)method was proposed.The water samples were concentrated and purified using HLB solid phase extraction columns.Based on the QuEChERS technique,the sediment samples were cleaned up with 0.2 vol.%ammonia-acetonitrile as the extractant and C18 and primary secondary amine(PSA)as sorbents.Under the optimal conditions,the separation of compounds was carried out on a Phenomenex Kinetex C18 column(100 mm×2.1 mm,particle size of 2.6 μm)using gradient elution with 5 mmol·L-1 ammonium acetate solution and acetonitrile as the mobile phase.The compounds were determined by UHPLC-MS/MS with ESI+source under MRM modes.The quantitative analysis was performed by an external standard approach.The compounds of avermectin and ivermectin could be examined within 7.5 min.Under the optimal conditions,the calibration curves were linear in the range of 1~100 μg·L-1.The recoveries spiked in blank water samples at four levels(0.05,0.5,2.5,and 5.0 μg·L-1)were in the range of 71.6%~88.2%,with the relative standard deviation(RSD,n=6)being 1.51%~8.81%.The limit of detection(LOD)was 0.02 μg·L-1 and the limit of quantification(LOQ)was 0.05 μg·L-1.The recoveries spiked in blank sediment sam-ples at four levels(1.0,10.0,50.0,100.0 ng·g-1)were in the range of 75.3%~96.4%,with the RSD(n=6)being 3.45%~8.99%.The LOD was 0.3 ng·g-1 and the LOQ was 1.0 ng·g-1.The developed approach is sensitive and accurate,suitable for determining avermectin and ivermectin in water and sediment from the aquaculture envi-ronment.

ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)avermectinivermectinwatersedimentaquaculture environment

万译文、杨霄、谢仲桂、索纹纹、陈湘艺、肖维、李小玲

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湖南省水产科学研究所,中国 长沙 410153

农业农村部渔业产品质量监督检验测试中心(长沙),中国 长沙 410153

超高效液相色谱-串联质谱 阿维菌素 伊维菌素 底泥 水产养殖环境

湖南省地方标准制定项目

2022-121

2024

湖南师范大学自然科学学报
湖南师范大学

湖南师范大学自然科学学报

CSTPCD北大核心
影响因子:0.62
ISSN:1000-2537
年,卷(期):2024.47(2)
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