固相萃取-高效液相色谱-紫外检测土壤中多西环素

doi:10.16431/j.cnki.1671-7236.2020.12.042

中国畜牧兽医 ›› 2020, Vol. 47 ›› Issue (12): 4174-4180.doi: 10.16431/j.cnki.1671-7236.2020.12.042

• 环境安全 • 上一篇

固相萃取-高效液相色谱-紫外检测土壤中多西环素

徐向月^1,2, 马文瑾^1,2, 安博宇^1,2, 王涵宇^1,2, 程古月^1,2, 刘振利^1,2, 黄玲利^1,2

1. 华中农业大学, 农业农村部畜禽产品质量安全风险评估实验室(武汉), 武汉 430070;
2. 华中农业大学, 国家兽药残留基准实验室, 农业农村部食品兽药残留检测重点实验室, 武汉 430070

收稿日期:2020-05-21 出版日期:2020-12-20 发布日期:2020-12-18
通讯作者: 黄玲利 E-mail:huanglingli@mail.hazu.edu.cn
作者简介:徐向月(1996-),女,河南登封人,硕士,研究方向:兽药环境安全性评价,E-mail:121813005@qq.com
基金资助:
"十三五"国家重点研发计划课题"抗菌药物代谢转归及环境微生物风险评估"（2018YTD0500301）

Detection of Doxycycline in Soil Using Solid Phase Extraction and High Performance Liquid Chromatography-Ultraviolet

XU Xiangyue^1,2, MA Wenjin^1,2, AN Boyu^1,2, WANG Hanyu^1,2, CHENG Guyue^1,2, LIU Zhenli^1,2, HUANG Lingli^1,2

1. Laboratory for Risk Assessment of Quality and Safety of Livestock and Poultry Products(Wuhan), Ministry of Agriculture and Rural Affairs, Huazhong Agricultural Univeristy, Wuhan 430070, China;
2. Key Laboratory for Detection of Veterinary Drug Residues of Ministry of Agriculture and Rural Affairs, National Reference Laboratory of Veterinary Drug Residues, Huazhong Agricultural Univeristy, Wuhan 430070, China

Received:2020-05-21 Online:2020-12-20 Published:2020-12-18

摘要/Abstract

摘要： 为了了解多西环素（DOX）在土壤中的污染现状，降低检测成本，本研究建立了固相萃取-高效液相色谱-紫外（HPLC-UV）检测3种土壤中DOX的分析方法。土壤样品通过采用乙腈和Na₂EDTA-Mcllvaine（1：1，V/V，pH 4.88）的混合溶液作为提取试剂，HLB固相萃取小柱进行富集净化，Agilent ZORBAX SB-C18（4.6 mm×250 mm×5 μm）色谱柱分离，以0.01 mol/L草酸（A）、乙腈（B）和甲醇（C）为流动相系统，在355 nm波长下进行高效液相色谱检测时提取效果最佳。以3倍信噪比确定方法检测限，以10倍信噪比确定方法定量限。结果表明，DOX在10 min出峰，在0.1~10 μg/mL范围内，DOX的峰面积与浓度线性关系良好，回归方程为y=22 747x+3.3256，相关系数是0.9999。本方法DOX的检测限为0.05 mg/kg，定量限为0.1 mg/kg。当土壤添加浓度为0.1 μg/g时，DOX在壤土、砂壤土及砂土中的回收率分别为58.96%、75.84%和83.06%，变异系数为1.00%~9.54%；当土壤添加浓度为0.2 μg/g时，DOX在壤土、砂壤土及砂土中的回收率分别为63.89%、70.48%和81.07%，变异系数为2.40%~8.83%；当土壤添加浓度为0.4 μg/g时，DOX在壤土、砂壤土及砂土中的回收率分别为59.02%、76.16%和81.29%，变异系数为1.52%~5.89%。本检测方法高效、稳定、特异性好，可以用于不同类型土壤中DOX的检测与定量，有助于环境中DOX检测方法的建立。

关键词: 土壤; 多西环素; 固相萃取; 高效液相色谱; 紫外

Abstract: In order to investigate the pollution status of DOX in soil and reduce the detection cost,a detection method of DOX in three soils was established by solid phase extraction and high performance liquid chromatography (HPLC-UV) in this study.The mixture of acetonitrile and Na₂EDTA-Mcllvaine (1:1,V/V) was used as extraction reagent for soil samples.HLB solid phase extraction column was used for enrichment and purification.Agilent ZORBAX SB-C18 (4.6 mm×250 mm×5 μm) column was used for separation.0.01 mol/L oxalic acid (A),acetonitrile (B) and methanol (C) were used as mobile phase system for HPLC detection at 355 nm.The limit of detection (LOD) was determined by 3 times S/N and the limit of quantitation (LOQ) was determined by 10 times S/N.The results showed that DOX peaked in 10 min.In the range of 0.1-10 μg/mL,the linear relationship between the peak area of DOX and the concentration was good.The regression equation was y=22 747x+3.3256,and the correlation coefficient was 0.9999.The LOD and LOQ of DOX in this method were 0.05 and 0.1 mg/kg,respectively.When the added concentration of DOX was 0.1 μg/g in soil,the recoveries of DOX in loam,sandy loam and sandy were 58.96%,75.84% and 83.06%,respectively,and the coefficient of variation(CV) was 1.00%-9.54%.The recoveries of DOX in loam,sandy loam and sandy were 63.89%,70.48% and 81.07%,respectively,and the CV 2.40%-8.83% when added 0.2 μg/g.The recoveries of DOX in loam,sandy loam and sandy soil was 59.02%,76.16% and 81.29% respectively,and the CV was 1.52%-5.89% when added 0.4 μg/g.This method was efficient,stable and specific.It could be used for the detection and quantification of DOX in different types of soil,which was helpful for the establishment of the detection method of DOX in the environment.

Key words: soil; doxycycline; solid phase extraction; high performance liquid chromatography; ultraviolet

中图分类号:

S859.7

徐向月, 马文瑾, 安博宇, 王涵宇, 程古月, 刘振利, 黄玲利. 固相萃取-高效液相色谱-紫外检测土壤中多西环素[J]. 中国畜牧兽医, 2020, 47(12): 4174-4180.

XU Xiangyue, MA Wenjin, AN Boyu, WANG Hanyu, CHENG Guyue, LIU Zhenli, HUANG Lingli. Detection of Doxycycline in Soil Using Solid Phase Extraction and High Performance Liquid Chromatography-Ultraviolet[J]. China Animal Husbandry and Veterinary Medicine, 2020, 47(12): 4174-4180.

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固相萃取-高效液相色谱-紫外检测土壤中多西环素

Detection of Doxycycline in Soil Using Solid Phase Extraction and High Performance Liquid Chromatography-Ultraviolet

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