采用多残留高效液相色谱法同时测定牛和猪肌肉、肝脏及肾脏组织中的七种青霉素。

Simultaneous determination of seven penicillins in muscle, liver and kidney tissues from cattle and pigs by a multiresidue high-performance liquid chromatographic method.

作者信息

Sørensen L K, Snor L K, Elkaer T, Hansen H

机构信息

Steins Laboratorium, Brørup, Denmark.

出版信息

J Chromatogr B Biomed Sci Appl. 1999 Nov 12;734(2):307-18. doi: 10.1016/s0378-4347(99)00389-8.

DOI:10.1016/s0378-4347(99)00389-8

PMID:10595728

Abstract

A high-performance liquid chromatographic (HPLC) method based on solid-phase extraction (SPE) was developed for determination of amoxicillin, penicillin G (benzylpenicillin), ampicillin, oxacillin, cloxacillin, nafcillin and dicloxacillin in muscle, liver and kidney tissues of pigs and cattle. The compounds were extracted in aqueous solution by precipitation of organic materials with a mixture of sulphuric acid and sodium tungstate. The extract was cleaned up by SPE on a divinylbenzene-co-N-vinylpyrrolidone polymeric sorbent. Further clean-up was performed by liquid-liquid partition with diethyl ether. The extract was derivatised with benzoic anhydride and 1,2,4-triazole mercury (II) reagent. Chromatography was performed by reversed-phase gradient HPLC on a C18 column with ultraviolet detection at 323 nm. The limits of detection estimated by a conservative model were in the range 8.9-11.1 microg/kg for amoxicillin, penicillin G, ampicillin, oxacillin, cloxacillin and nafcillin and 18.3-20.9 microg/kg for dicloxacillin. The mean recovery range was 66-77% for amoxicillin, 73-75% for penicillin G, 81-82% for ampicillin, 73-76% for oxacillin, 74-75% for cloxacillin, 66-72% for nafcillin and 58-65% for dicloxacillin.

摘要

建立了一种基于固相萃取（SPE）的高效液相色谱（HPLC）方法，用于测定猪和牛肌肉、肝脏及肾脏组织中的阿莫西林、青霉素G（苄青霉素）、氨苄西林、苯唑西林、氯唑西林、萘夫西林和双氯西林。通过用硫酸和钨酸钠的混合物沉淀有机物质，将化合物从水溶液中萃取出来。萃取液用二乙烯基苯 - 共 - N - 乙烯基吡咯烷酮聚合物吸附剂进行固相萃取净化。通过用乙醚进行液 - 液分配进一步净化。萃取液用苯甲酸酐和1,2,4 - 三唑汞（II）试剂衍生化。采用反相梯度HPLC在C18柱上进行色谱分析，紫外检测波长为323nm。通过保守模型估算的检测限，阿莫西林、青霉素G、氨苄西林、苯唑西林、氯唑西林和萘夫西林为8.9 - 11.1μg/kg，双氯西林为18.3 - 20.9μg/kg。阿莫西林的平均回收率范围为66 - 77%，青霉素G为73 - 75%，氨苄西林为81 - 82%，苯唑西林为73 - 76%，氯唑西林为74 - 75%，萘夫西林为66 - 72%，双氯西林为58 - 65%。