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采用离线柱式样品净化和在线二极管阵列紫外-可见检测的肉类中氯霉素残留的高效液相色谱筛选和确证方法。

High-performance liquid chromatographic screening and confirmation methods for chloramphenicol residues in meat with off-line cartridge sample clean-up and on-line diode array UV-VIS detection.

作者信息

Keukens H J, Beek W M, Aerts M M

出版信息

J Chromatogr. 1986 Feb 21;352:445-53. doi: 10.1016/s0021-9673(01)83400-2.

DOI:10.1016/s0021-9673(01)83400-2
PMID:3700510
Abstract

Two high-performance liquid chromatography (HPLC) methods for the analysis and confirmation of residues of the antibiotic chloramphenicol in edible animal tissues are described. The first method consists of an aqueous extraction followed by purification through an Extrelut cartridge and toluene partition. With this simple and rapid method, meat samples can be screened at the 5 micrograms/kg level. The second, more comprehensive, method is based on ethyl acetate extraction, followed by purification through a silica Sep-Pak cartridge and partition with buffer-diethyl ether and water-toluene. Confirmation of positive peaks at the 10 micrograms/kg level is performed by diode array UV-VIS detection. The recoveries for the two methods at the 10 micrograms/kg level are 58 and 85% respectively, coefficients of variation 5-6%. With the confirmation method, glucuronide and sulphate conjugates can be determined. However, in a positive reference sample (pig) none was observed.

摘要

本文描述了两种用于分析和确证食用动物组织中抗生素氯霉素残留量的高效液相色谱(HPLC)方法。第一种方法包括水相萃取,随后通过Extrelut柱净化和甲苯分配。采用这种简单快速的方法,可在5微克/千克水平筛查肉类样品。第二种更全面的方法基于乙酸乙酯萃取,随后通过硅胶Sep-Pak柱净化,并用缓冲液 - 乙醚和水 - 甲苯进行分配。通过二极管阵列紫外 - 可见检测对10微克/千克水平的阳性峰进行确证。两种方法在10微克/千克水平的回收率分别为58%和85%,变异系数为5 - 6%。采用确证方法可测定葡萄糖醛酸和硫酸盐结合物。然而,在一个阳性参考样品(猪)中未观察到结合物。

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