鸡肉中11种喹诺酮类药物多残留的高效液相色谱检测

Multi-residue determination of 11 quinolones in chicken muscle by high performance liquid chromatography with fluorescence detection

建立了用荧光检测器同时测定11种喹诺酮类药物（包括诺氟沙星、培氟沙星、环丙沙星、恩诺沙星、氧氟沙星、达氟沙星、洛美沙星、二氟沙星、沙拉沙星、恶喹酸和氟甲喹）在鸡肉中的多残留的高效液相色谱检测方法。鸡肉样品用10%三氯乙酸-乙腈（体积比为7∶3）提取两次并稀释,随后用反相固相萃取柱净化。采用Hypersil BDS-C18色谱柱分离,以乙腈和水为流动相梯度洗脱,荧光检测器用程序编程检测波长检测。11种喹诺酮类药物标准曲线的线性范围为5~1 200μg/L,相关系数大于0.998。在高、中、低三个添加水平下的回收率为56%~119%,批内相对标准偏差为0.4%~16.1%,批间相对标准偏差为1.4%~23.0%。检出限和定量限分别为1~23μg/kg和4~40μg/kg。该方法快速、灵敏,达到了兽药残留检测的要求。

A high performance liquid chromatographic（HPLC） method with fluorescence detection was developed for the simultaneous determination of 11 quinolones（QNs）（norfloxacin,ofloxacin,ciprofloxacin,pefloxacin,lomefloxacin,danofloxacin,enrofloxacin,sarafloxacin,difloxacin,oxolinic acid and flumequine） residues in chicken muscle.The chicken muscle samples were extracted by 10% trichloroacetic acid/acetonitrile（7∶3,v/v） twice,diluted and cleaned up by a reversed-phase solid-phase extraction（SPE） cartridge.The QNs were separated on a reversed-phase C18 column（Hypersil BDS-C18） with mobile phase gradient elution（acetonitrile and water as mobile phases） and detected by a fluorescence detector with a wavelength program.The linear ranges of quinolone calibrations were 5-1200 μg/L in chicken muscle with the correlation coefficients more than 0.998.The recoveries for chicken muscle fortified with 11 QNs at three levels were 56%-119% with acceptable intra-batch relative standard deviations（RSD）（0.4%-16.1%） and inter-batch RSD（1.4%-23.0%）.The limits of detection（LOD） and limits of quantification（LOQ） were 1-23 μg/kg and 4-40 μg/kg for the 11 QNs,respectively.The sensitivity meets the quantification requirements for the residue analysis.