食用蚕蛹中酰胺醇类抗生素的残留量测定
Determination of Amidoxime Antibiotic Residues in Edible Silkworm Pupae
黄恺 1兰清滢 2韦娜 1刘玉雯 1杨昆 1汪文龙 1司露露 1秦富1
作者信息
- 1. 南宁海关技术中心 南宁 530201
- 2. 南宁师范大学 南宁 530100
- 折叠
摘要
本文建立了检测食用蚕蛹中氯霉素、甲砜霉素、氟苯尼考和氟苯尼考胺 4 种酰胺醇类抗生素残留量的液相色谱-串联质谱方法.试样用 1%氨水乙腈提取,无水乙酸钠和无水硫酸镁除水,C18 吸附剂净化,氮吹干后用纯水复溶.采用0.05%氨水水溶液和甲醇为流动相,经Eclipse Plus C18(2.1 mm×100 mm,1.8 μm)色谱柱分离,在电喷雾离子源正、负离子模式下进行多反应监测(MRM),用同位素内标法定量.实验结果显示,氯霉素在 0.025～1.000 μg/L浓度范围内线性相关性良好,相关系数r为0.9990,加标平均回收率为99.1%～108.6%,相对标准偏差(RSDs)为3.3%～7.0%.甲砜霉素、氟苯尼考和氟苯尼考胺在 0.125～5.000 μg/L浓度范围内线性相关性良好,相关系数r≥0.9920,加标平均回收率为 89.5%～112.1%,相对标准偏差(RSDs)为 3.6%～15.8%.该方法快速、准确,灵敏,适用于食用蚕蛹中氯霉素、甲砜霉素、氟苯尼考和氟苯尼考胺的残留检测.
Abstract
A liquid chromatography-tandem mass spectrometry(LC-MS/MS)method was established for the determination of residues of four acylamide antibiotics,namely chloramphenicol,thiamphenicol,florfenicol and florfenicol amine in edible silkworm pupae.The samples were extracted with acetonitrile containing 1%ammonia water,dehydrated with anhydrous sodium acetate and anhydrous magnesium sulfate,purified with C18 adsorbent,and dissolved in pure water after nitrogen drying.The target compounds were separated by Eclipse Plus C18(2.1 mm×100 mm,1.8 μm)chromatographic column under the mobile phase of 0.05%ammonia aqueous solution and methanol,detected by multi-reaction monitoring(MRM)under positive and negative ion modes of electric spray ion source,and quantitative analyzed by isotope internal standard method.The experimental results show that chloramphenicol had a good linear correlation in the concentration range of 0.025-1.000 μg/L.The correlation coefficient(r)was 0.9990.The average recovery rate of chloramphenicol was 99.1%-108.6%,and the relative standard deviations(RSDs)were 3.3%-7.0%.Thiamphenicol,florfenicol and florfenicol amine had a good linear correlation in the concentration range of 0.125 μg/L to 5.000 μg/L.The correlation coefficients were≥0.9920.Their average recovery rates were 89.5%-112.1%,and RSDs were 3.6%-15.8%.This method offers rapid,accurate,and sensitive detection,making it suitable for the analysis of the aforementioned antibiotics in edible silkworm pupae.
关键词
蚕蛹/酰胺醇类抗生素/氯霉素/氟苯尼考胺Key words
silkworm pupae/amide alcohol antibiotics/chloramphenicol/florfenicol amine引用本文复制引用
基金项目
南宁市科学研究与技术开发计划项目(20212148)
出版年
2024
NETL
NSTL
万方数据