建立一种采用液相色谱-紫外可见检测法测定牛乳中青霉素G，并通过质谱检测进行确证的分析方法。

Development of an analytical method for penicillin G in bovine milk by liquid chromatography with ultraviolet-visible detection and confirmation by mass spectrometric detection.

作者信息

Tyczkowska K, Voyksner R D, Aronson A L

机构信息

Department of Anatomy, Physiological Sciences and Radiology, College of Veterinary Medicine, North Carolina State University, Raleigh 27606.

出版信息

J Chromatogr. 1989 May 5;490(1):101-13. doi: 10.1016/s0378-4347(00)82765-6.

DOI:10.1016/s0378-4347(00)82765-6

PMID:2760143

Abstract

A liquid chromatographic (LC) method with ultraviolet-visible photodiode array (UV-VIS PDA) detection was developed to measure penicillin G in bovine milk. A liquid chromatographic-mass spectrometric (LC-MS) procedure was divised to confirm the LC method. The method involved diluting milk with a drug-releasing solvent consisting of acetonitrile-methanol-water and ultrafiltration through a 10,000 dalton cutoff filter. Penicillin G was separated from other components in the ultrafiltrate by ion-paired LC using a reversed-phase microbore column eluted with a 25% acetonitrile solution. The LC method was confirmed by thermospray LC-MS. The detection limit for penicillin G determination in milk was estimated to be 10 ppb for LC with UV-VIS PDA and 100 ppb for LC-MS.

摘要

建立了一种采用紫外-可见光电二极管阵列（UV-VIS PDA）检测的液相色谱（LC）方法来测定牛乳中的青霉素G。设计了一种液相色谱-质谱（LC-MS）方法来确证该LC方法。该方法包括用由乙腈-甲醇-水组成的药物释放溶剂稀释牛奶，并通过截留分子量为10000道尔顿的滤膜进行超滤。在超滤液中，青霉素G通过离子对LC，使用反相微径柱，用25%乙腈溶液洗脱，与其他成分分离。通过热喷雾LC-MS确证了该LC方法。对于牛奶中青霉素G的测定，LC结合UV-VIS PDA的检测限估计为10 ppb，LC-MS的检测限为100 ppb。