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当前位置: 首页 > 文章 > 液质联用测定乌鸡中氟喹诺酮的方法对比 饲料博览 2017 (3) 6-9
Position: Home > Articles > LC-MS Method of Determination of Fluoroquinolone in Silkie Feed Review 2017 (3) 6-9

液质联用测定乌鸡中氟喹诺酮的方法对比

作  者：
徐少华;闫清华;刘国华;罗燕;谭磊
单  位：
深圳市农产品质量安全检验检测中心
关键词：
液相质谱;氟喹诺酮;前处理;阳性样品;乌鸡
摘  要：
以液相色谱-质谱/质谱法为基础,在试验前处理方面进行了优化,通过添加回收试验和阳性样品检测,对比液相色谱-质谱/质谱法和优化后的前处理两种方式试验的结果。优化的前处理过程:称取试样3.0 g,加入提取液10 m L,经球磨机研磨,超声波辅助提取,冷冻离心。移取上清液过固相萃取柱,移取净化液3.00 m L氮吹至0.5 m L,加入流动相定容,过0.22μm膜上机。10、50、100、200、800、5 000μg·kg~(-1)6个浓度建立标准曲线,相关系数R均>0.998。回收率试验10、50、200μg·kg~(-1)3个浓度对比,回收率范围为85.6%~102.2%,RSD≤3.92%。20份不同浓度阳性样品,两种方法检测值的相对标准偏差为0.67%~19.6%。优化后的前处理方法不但操作简单,省时省力,大幅降低检测成本,而且测定值稳定可靠,可提高大批量鸡肉中氟喹诺酮类药物的阳性筛选效率。
译  名：
LC-MS Method of Determination of Fluoroquinolone in Silkie
作  者：
XU Shaohua;YAN Qinghua;LIU Guohua;LUO Yan;TAN Lei;Shenzhen Agricultural Product Quality Safety Inspection Testing Center;
关键词：
liquid mass spectrometry;;fluoroquinolone;;preliminary treatment;;positive samples;;silkie
摘  要：
Based on liquid chromatography mass spectrometry/mass spectrometry, the test pretreatment was opti-mized, by adding the recycling experiment and positive samples test, compared with liquid chromatography mass spec-trometry/mass spectrometry and the optimized pretreatment results. Optimization of pretreatment process: took sample3.0 g adding extract 10 m L, grinding by ball mill, ultrasonic assisted extraction and refrigerated centrifuge. Moving theclear liquid to the solid phase extraction column, the purified liquid 3.00 m L nitrogen blowing to 0.5 m L, adding mo-bile phase capacitance over 0.22 um membrane computer. Test selected 10, 50, 100, 200, 800, 5 000 u g·kg~(-1)six lev-els to establish standard curve, correlation coefficient R was greater than 0.998. Recovery experiment was 10, 50, 200ug·kg~(-1)three concentrations of contrast, recovery range 85.6%~102.2%, RSD 3.92% or less. Twenty different concen-tration positive sample of the two methods, relative standard deviation was between 0.67%~19.6%. The optimized pre-treatment method was not only the operation simple, save time and effort, greatly reduce the testing cost, and stableand reliable measurements. The method could improve the mass of the chicken positive screening efficiency.

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