液相色谱法测定动物脂肪中的孕激素

Liquid chromatographic determination of progestogens in animal fat.

作者信息

Andresen M T, Fesser A C

机构信息

Agriculture Canada, Health of Animals Laboratory, Saskatoon, SK, Canada.

出版信息

J AOAC Int. 1996 Sep-Oct;79(5):1037-42.

PMID:8823911

Abstract

A liquid chromatographic method was developed for determination of 3 progestogens-melengestrol acetate, megestrol acetate, and chlormadinone acetate-found in edible tissue at concentrations between 10 and 1000 ppb. These progestogens are commonly used as feed additives to control herd estrus and to improve feed efficiency. Rendered fat was extracted with acetonitrile, washed with hexane, and dried. The remaining lipids were saponified with sodium hydroxide and precipitated with magnesium chloride. The progestogens were extracted from the basic solution with hexane, dried, and cleaned up on a cyanopropyl solid-phase extraction column in the normal-phase mode. The eluate was dried and reconstituted with acetonitrile-water (7 + 3, v/v). Chromatography was performed on a 5 microns high-carbon load C18 column with acetonitrile-water (7 + 3, v/v) at 1 mL/min and UV detection at 291 nm. Recoveries from fortified samples ranged from 84 to 116%. The limit of quantitation was 10 ppb for both beef and pork. The detection limit was 3 ppb.

摘要

建立了一种液相色谱法，用于测定在可食用组织中浓度介于10至1000 ppb之间的3种孕激素——醋酸美仑孕酮、醋酸甲地孕酮和醋酸氯地孕酮。这些孕激素通常用作饲料添加剂，以控制畜群发情并提高饲料效率。用乙腈提取炼过的脂肪，用己烷洗涤并干燥。剩余的脂质用氢氧化钠皂化，并用氯化镁沉淀。用己烷从碱性溶液中提取孕激素，干燥后，以正相模式在氰丙基固相萃取柱上进行净化。洗脱液干燥后，用乙腈 - 水（7 + 3，v/v）复溶。在5微米高碳载量C18柱上进行色谱分析，流动相为乙腈 - 水（7 + 3，v/v），流速为1 mL/min，在291 nm处进行紫外检测。加标样品的回收率在84%至116%之间。牛肉和猪肉的定量限均为10 ppb。检测限为3 ppb。