福建畜牧兽医
福建畜牧獸醫
복건축목수의
FUJIAN JOURNAL OF ANIMAL HUSBANDRY AND VETERINARY
2015年
2期
28-29,30
,共3页
管祖东%吕小玲%李文迹%罗忠宝
管祖東%呂小玲%李文跡%囉忠寶
관조동%려소령%리문적%라충보
液相色谱串联质谱%氯霉素%残留%鸡肉%鸡蛋
液相色譜串聯質譜%氯黴素%殘留%鷄肉%鷄蛋
액상색보천련질보%록매소%잔류%계육%계단
HPLC-MS/MS%chloramphenicols%residue%chicken%eggs
建立了鸡肉、鸡肝和鸡蛋中氯霉素的高效液相色谱串联质谱测定方法,试样经三氯乙酸除蛋白及乙酸乙酯液液萃取提取和净化后,C18柱HPLC进行分离,多反应选择离子检测。方法的回收率和变异系数分别在80%~110%和8%~10%。该方法对鸡肉中氯霉素检测限为0.1μg/kg。
建立瞭鷄肉、鷄肝和鷄蛋中氯黴素的高效液相色譜串聯質譜測定方法,試樣經三氯乙痠除蛋白及乙痠乙酯液液萃取提取和淨化後,C18柱HPLC進行分離,多反應選擇離子檢測。方法的迴收率和變異繫數分彆在80%~110%和8%~10%。該方法對鷄肉中氯黴素檢測限為0.1μg/kg。
건립료계육、계간화계단중록매소적고효액상색보천련질보측정방법,시양경삼록을산제단백급을산을지액액췌취제취화정화후,C18주HPLC진행분리,다반응선택리자검측。방법적회수솔화변이계수분별재80%~110%화8%~10%。해방법대계육중록매소검측한위0.1μg/kg。
A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the quan﹣titative determination of chloramphenicols respectively in the chicken and liver of chicken and eggs. The chloramphenicols in eggs were deproteinated with acetocaustin acid and acetic ether followed by liquid-liquid extraction.Further clean-up was performed by solid phase extraction(SPE) through mixed mode columns (PEP SPE).The separation of the compounds was carried on a Agilent Eclipse Plus C18 column (C18, 3.5 μm×100 mm×2.1 mm(id) by a gradient elution using acetonitrile and 0.1% formic acid as mobile phases. The analytes were detected by tandem mass spectrometry in multiple reaction monitoring (MRM) mode with negative electrospray ion﹣ization.The chloramphenicols quantified by internal standard method.The linear ranges were 0.1~20. 0 μg/L and the correlation coeffi﹣cients were not less than 0.9995.The average recoveries and relative standard deviations ranged from80%-110%and 8%~10%respec﹣tively at the spiked levels of 0.1,0.2 and 1.0 μg/kg for the both markers. The limit of quantitation (LOQ) was 0.1 μg/kg.The method is sensitive,accurate and suitable for the determination and confirmation of chloramphenicols in chicken and eggs.