HPLC检测猪血浆和尿液中的喹烯酮及其主要代谢物

本试验旨在建立猪血浆和猪尿液中喹烯酮及其主要代谢物3-甲基-喹噁啉-2-羧酸(MQCA)、脱一氧喹烯酮、脱二氧喹烯酮同时检测的高效液相色谱法。血浆样品用乙腈沉淀蛋白,经高速离心后直接检测。尿液样品用乙酸乙酯提取喹烯酮、脱一氧喹烯酮、脱二氧喹烯酮,用盐酸提取MQCA,再用乙酸乙酯萃取,50 ℃氮气吹干后过HLB固相萃取小柱。以0.1%甲酸水-乙腈为流动相梯度洗脱,314 nm波长下检测。喹烯酮及3种代谢物在血浆中的回收率在72.54%~104.2%之间,尿液中的回收率在63.20%~86.24%之间。4种目标化合物在血浆和尿液中定量限均为0.05 μg/mL。

Determination of Quinocetone and its Main Metabolites in Porcine Plasma and Urine by HPLC

A HPLC method was developed for simultaneous determination of quinocetone and its three main metabolites in porcine plasma and urine. Plasma samples were extracted with acetonitrile and determined after high speed centrifugation. Quinocetone, demonoxyquinocetone and desoxyquinocetone were extracted with ethylacetate from urine samples. MQCA were extracted with hydrochloric acid, ethylacetate, then dried under nitrogen at 50 ℃ and cleaned up by SPE column. Mobile phase consisted of acetonitrile and 0.1% formic acid was used for gradient elution under the detective wavelength of 314 nm. The recoveries of quinocetone and its three main metabolites in plasma were 72.54% to 104.2% and 63.20% to 86.24% in urine. The limit of quantitation of these four target compounds in plasma and urine was 0.05 μg/mL.