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基于分散固相萃取和冻干的超高效液相色谱-串联质谱法分析鸡粪和环境水中的 authorized coccidiostats

Analysis of authorized coccidiostats in chicken feces and environmental water by ultra-performance liquid chromatography-tandem mass spectrometry based on dispersive solid-phase extraction and lyophilization.

机构信息

Laboratory of Animal Genetics, Breeding and Reproduction in the Plateau Mountainous Region, Ministry of Education, Guizhou University, Guiyang 550025, Guizhou Province, China.

Laboratory of Animal Genetics, Breeding and Reproduction in the Plateau Mountainous Region, Ministry of Education, Guizhou University, Guiyang 550025, Guizhou Province, China; Bureau of Agriculture and Rural Areas of Kaili City, Kaili 556000, Guizhou Province, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2023 Sep 1;1229:123884. doi: 10.1016/j.jchromb.2023.123884. Epub 2023 Sep 9.

DOI:10.1016/j.jchromb.2023.123884
PMID:37714049
Abstract

A simple, sensitive, and efficient method based on ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the determination of 8 coccidiostats in chicken feces and environmental water (including sewage, pond water, and lake water) surrounding the farm. Target analytes in chicken feces were extracted with 2% acetic acid in acetonitrile solution, followed by a dispersive solid-phase extraction (DSPE) cleanup step using the mixture of PSA and C adsorbents. Environmental water samples were pretreated using a lyophilization approach. Analysis was carried out on a UPLC-MS/MS with the combination of methanol and 0.1% formic acid aqueous solution as the mobile phase under multiple reaction monitoring in positive and negative ionization modes. Results showed that 8 coccidiostats were linear with correlation coefficients higher than 0.99. Method validation was performed using fortified samples, reaching satisfactory recoveries of 75.9%-97.8% in chicken feces and 71.9%-108.2% in environmental water. Limits of detection for 8 analytes in chicken feces and environmental water were 0.03∼2 µg/kg and 0.005∼1 µg/L, respectively. Matrix effects were calculated and strong signal suppression (>50%) for some coccidiostats was observed. The developed method was successfully applied to analyze coccidiostats in chicken feces and environmental water collected from local chicken farms.

摘要

建立了一种基于超高效液相色谱-串联质谱(UPLC-MS/MS)的简单、灵敏、高效的方法,用于检测鸡粪和农场周围环境水中(包括污水、池塘水和湖水)的 8 种抗球虫药。鸡粪中的目标分析物用 2%乙酸在乙腈溶液中提取,然后用 PSA 和 C 吸附剂的混合物进行分散固相萃取(DSPE)净化。环境水样采用冻干法预处理。采用甲醇和 0.1%甲酸水溶液作为流动相,在正负离子模式下进行多反应监测,在 UPLC-MS/MS 上进行分析。结果表明,8 种抗球虫药均呈线性,相关系数均高于 0.99。采用加标样品进行方法验证,在鸡粪中的回收率为 75.9%-97.8%,在环境水中的回收率为 71.9%-108.2%,均达到满意的效果。8 种分析物在鸡粪和环境水中的检测限分别为 0.03∼2μg/kg 和 0.005∼1μg/L。计算了基质效应,发现一些抗球虫药存在强烈的信号抑制(>50%)。该方法成功应用于检测当地鸡场鸡粪和环境水中的抗球虫药。

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