Objective To explore the cause of lower recovery inAnnouncementNo.781of the ministry of agriculture the determination of quinolones residues in egg by high performance liquid chromatography Method. Methods The samples were extracted with n-hexane and purified by the C18 solid phase extraction column. The study on the influence factor of lower recovery in the detection of fluoroquinolones residues in eggs were conducted from the following aspects: different solid phase extraction column models, mobile phase elution volume, water elution volume, n-hexane extraction times and agitation ways.ResultsThe recoveries of fluoroquinolones residues in eggs were influenced by the factors selected in this study. One time of n-hexane extraction decreased the recovery of ciprofloxacin from 97.5% to 35.2%, danofloxacin from 92.5% to 32.9%, enrofloxacin from 88.1% to 76.4%, and sarafloxacin from 85.6% to 37.4%. The use of ordinary oscillator decreased the recovery of ciprofloxacin from 12.3% to 0 and enrofloxacin from 25.7% to 7.3%.ConclusionThe n-hexane extraction and use of ordinary oscillator are the main causes of lower recovery inAnnouncementNo.781of the ministry of agriculture the determination of quinolones residues in egg by high performance liquid chromatography Method.%目的：探讨《农业部781号公告-6-2006鸡蛋中氟喹诺酮类药物残留量的测定高效液相色谱法》中方法回收率较低的原因。方法样品用正己烷提取后,采用 C18固相萃取柱进行净化,对不同的固相萃取柱型号、流动相洗脱用量、水洗脱用量、正己烷萃取次数和振荡方式对空白试剂样品中氟喹诺酮类药物的回收率进行研究,探讨影响回收率的因素。结果本研究选取的因素对氟喹诺酮类药物的回收率均有影响,其中1次正己烷脱脂过程使环丙沙星的回收率从97.5%降至35.2%,达氟沙星从92.5%降至32.9%,恩诺沙星从88.1%降至76.4%,沙拉沙星从85.6%降至37.4%。普通振荡器振荡使环丙沙星的回收率从12.3%降至0,恩诺沙星的回收率从25.7%降至7.3%,沙拉沙星的回收率从13%降至0。结论正己烷脱脂及普通振荡器振荡是《农业部781号公告-6-2006鸡蛋中氟喹诺酮类药物残留量的测定高效液相色谱法》中方法回收率较低的主要原因。
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