福建畜牧兽医
福建畜牧獸醫
복건축목수의
FUJIAN JOURNAL OF ANIMAL HUSBANDRY AND VETERINARY
2015年
2期
18-19,20
,共3页
吕小玲%管祖东%黄丽琴%李文迹%罗忠宝
呂小玲%管祖東%黃麗琴%李文跡%囉忠寶
려소령%관조동%황려금%리문적%라충보
液相色谱串联质谱%环丙沙星%残留
液相色譜串聯質譜%環丙沙星%殘留
액상색보천련질보%배병사성%잔류
high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS)%ciprofloxacin%residue chicken
建立了鸡肉中环丙沙星的高效液相色谱串联质谱测定方法,试样经 EDTA-Na缓冲盐提取和净化后,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90%~110%和3%~10%。该方法对鸡肉中环丙沙星检测限为1μg/kg。
建立瞭鷄肉中環丙沙星的高效液相色譜串聯質譜測定方法,試樣經 EDTA-Na緩遲鹽提取和淨化後,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90%~110%和3%~10%。該方法對鷄肉中環丙沙星檢測限為1μg/kg。
건립료계육중배병사성적고효액상색보천련질보측정방법,시양경 EDTA-Na완충염제취화정화후,C18주HPLC진행분리,다반응선택리자검측。방법적회수솔화변이계수분별재90%~110%화3%~10%。해방법대계육중배병사성검측한위1μg/kg。
A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS /MS) method was developed for the quantitative determination of Ciprofloxacin respectively in the chicken. The ciprofloxacin in chicken were deproteinated with EDTA-Na Mcllvaine buffer followed by liquid-liquid extraction. Further clean-up was performed by solid phase extraction (SPE) through mixed mode columns (PEP-2 SPE). The separation of the compounds was carried on a Agilent Eclipse Plus C18 column (C18, 3.5μm× 100 mm×2.1 mm(id) by a gradient elution using 0.1%formic acid acetonitrile and 0.1%formic acid water as mobile phases. The analyzes were detected by tandem mass spectrometry in multiple reaction monitoring (MRM) mode with negative electrospray ioniza﹣tion. The ciprofloxacin quantified by internal standard method. The linear ranges were 1.0~20.0 μg/L and the correlation coefficients were not less than 0.992. The average recoveries and relative standard deviations ranged from90%~110%and 3%~10%respectively at the spiked levels of 1,2 and 10 μg/kg for the both markers. The limit of quantitation (LOQ) was 1 μg/kg. The method is sensitive,ac﹣curate and suitable for the determination and confirmation of chloramphenicols in chicken and eggs.