首页|QuEChERS-HPLC-MS/MS法检测蚕砂中氯霉素残留量

QuEChERS-HPLC-MS/MS法检测蚕砂中氯霉素残留量

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本文建立了一种QuEChERS和C18固相萃取柱净化结合液相色谱串联质谱方法测定蚕砂中氯霉素残留.经乙酸乙酯提取,GCB和C18固相萃取柱净化,以甲醇和水为流动相梯度洗脱,C18柱(2.1 mm×100mm,1.7μm)分离,在电喷雾离子源(ESI)负离子模式下采用液相色谱-串联质谱仪测定,内标法定量.结果显示,在0.02μg/L~5.00μg/L,氯霉素具有良好的线性关系,相关系数为1.000.氯霉素在4个加标水平(0.1 μg/kg、0.3 μg/kg、1.0 μg/kg、2.0 μg/kg)下回收率范围为74.7%~103.0%,RSD在4.36%~9.64%.该方法操作快速简单,且灵敏度与回收率高,可用于蚕砂中氯霉素残留的检测分析.
Determination of chloramphenicol residues in silkworm excrement-high performance liquid chromatography-tandem mass spectrometry method with QuEChERS
A method for the determination of chloramphenicol residues in silkworm excrement based on QuEChERS-High Performance liquid chromatography-tandem mass spectrometry was developed.The method was extracted by ethyl acetate,pu-rified by GCB and C18 solid phase extraction column,eluted by methanol and water as mobile phase gradient,separated by C18 column(2.1 mm×100mm,1.7 μm),determined by liquid chromatography tandem mass spectrometry under the negative ion mode of electric spray ion source(ESI),and quantified by internal standard method.The results showed that chloramphenicol had a good linear relationship between 0.02 μg/L-5.00 μg/L with a correlation coefficient of 1.000.The recoveries of chlo-ramphenicol at four supplemental levels(0.1 μg/kg,0.3 μg/kg,1.0 μg/kg,2.0 μg/kg)ranged from 74.7%-103.0%,and the RSD ranged from 4.36%-9.64%.The method is quick,simple,sensitive and has high recovery rate,so it can be used for the de-tection and analysis of chloramphenicol residues in silkworm excrement.

Silkworm excrementChloramphenicolQuEChERSSolid phase extractionHigh performance liquid chromatogra-phy-tandem mass spectrometry

梁香、崔凤云、朱绍华、付善良、成婧、陆静、焦艳娜

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长沙海关技术中心&食品安全科学技术湖南省重点实验室 湖南长沙 410004

中国海关科学技术研究中心

蚕砂 氯霉素 QuEChERS 固相萃取 液相色谱-串联质谱

海关总署科研项目

2023HK078

2024

质量安全与检验检测
中国检验检疫科学研究院

质量安全与检验检测

影响因子:0.399
ISSN:2096-8876
年,卷(期):2024.34(2)
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