高效液相色谱-电喷雾电离串联质谱法测定鸡肉、鸡蛋中氯霉素、甲砜霉素和氟苯尼考药物残留量

目的建立高效液相色谱-电喷雾电离串联质谱法测定鸡肉和鸡蛋中氯霉素、甲砜霉素、氟苯尼考残留量的分析方法。方法准确称取5 g样品,添加同位素内标氯霉素-d5后,乙腈提取,LC-Si硅胶小柱净化,正己烷进一步除脂,0.22μm滤膜过滤后高效液相色谱-电喷雾电离串联质谱测定。采用负离子电喷雾电离源,多反应监测（multiple reaction monitoring,MRM）模式。结果氯霉素、甲砜霉素和氟苯尼考在0.5~200μg/L的系列浓度范围内线性良好,其线性方程分别为Y=0.880X-0.215,Y=0.032X-0.076和Y=0.108X-0.115,相关系数r~2均大于0.990;方法的...

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Bibliographic Details
Published in食品安全质量检测学报 Vol. 8; no. 6; pp. 2211 - 2219
Main Author 张静 高玉时 周倩 万玉 唐梦君 唐修君 顾荣 陆俊贤 张小燕 陈大伟
Format Journal Article
LanguageChinese
Published 中国农业科学院家禽研究所,扬州,225125 2017
Subjects
氟苯尼考
氯霉素
甲砜霉素
高效液相色谱-电喷雾电离串联质谱法
鸡肉
鸡蛋
high performance liquid chromatography-electrospray ionization-tandem mass spectrometry
chicken
高效液相色谱-电喷雾电离串联质谱法
chlorampheincol
egg
鸡蛋
甲砜霉素
氟苯尼考
thiamphenicol
鸡肉
florfenicol
氯霉素
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Summary:目的建立高效液相色谱-电喷雾电离串联质谱法测定鸡肉和鸡蛋中氯霉素、甲砜霉素、氟苯尼考残留量的分析方法。方法准确称取5 g样品,添加同位素内标氯霉素-d5后,乙腈提取,LC-Si硅胶小柱净化,正己烷进一步除脂,0.22μm滤膜过滤后高效液相色谱-电喷雾电离串联质谱测定。采用负离子电喷雾电离源,多反应监测（multiple reaction monitoring,MRM）模式。结果氯霉素、甲砜霉素和氟苯尼考在0.5~200μg/L的系列浓度范围内线性良好,其线性方程分别为Y=0.880X-0.215,Y=0.032X-0.076和Y=0.108X-0.115,相关系数r~2均大于0.990;方法的检测限和定量限分别是0.05μg/kg和0.1μg/kg;在加标水平在0.1~5.0μg/kg的范围内,鸡肉基质中平均回收率在87.01%~117.8%之间,鸡蛋基质中平均回收率在80.74%~115.0%之间;方法的日内精密度相对标准偏差在4.02%~9.88%之间,日间精密度相对标准偏差在5.72%~12.78%之间。结论该方法简单易行,回收率好,灵敏度高,特异性好,能满足目前大多数日常检测和监督的需要。
Bibliography:Objective To establish a method for the determination of chlorampheincols （CAP）, thiamphenicol （TAP） and florfenicol （FF） residues in chicken and egg by high performance liquid chromatography-electrospray ionization- tandem mass spectrometry（HPLC-ESI-MS/MS）. Methods The 5 g sample was taken and added an isotope standard （CAP-d5）, then extracted with acetonitrile, cleaned up with LC-Si column, and degreased by hexane. The eluent was filtered through 0.22 um membrane and then analyzed by HPLC-ESI-MS/MS. Mass spectral acquisition was carried out by using electrospray ionization in negative ion mode with multiple reaction monitoring（MRM）. Results The calibration curves of mixed standard solution showed good linearities in the concentrations from 0.5 to 200 μg/L with the correlation coefficients （r2） more than 0.990. The linear equations of CAP, TAP and FF were Y=0.880X-0.215, Y=0.032X-0.076 and Y=0.108X-0.115, respectively. The limit of detection （LOD） and limit of quantification （LOQ） of the method were 0.05 μg/
ISSN:2095-0381