Lin Baoyin
Guangzhou Agricultural Standard and Supervisory Center, Guangzhou 510305, China.
Se Pu. 2009 Mar;27(2):206-10.
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% trichioroacetic 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 microg/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 microg/kg and 4-40 kg/kg for the 11 QNs, respectively. The sensitivity meets the quantification requirements for the residue analysis.
建立了一种带荧光检测的高效液相色谱（HPLC）方法，用于同时测定鸡肉中11种喹诺酮类药物（QNs）（诺氟沙星、氧氟沙星、环丙沙星、培氟沙星、洛美沙星、达氟沙星、恩诺沙星、沙拉沙星、二氟沙星、恶喹酸和氟甲喹）的残留量。鸡肉样品用10%三氯乙酸/乙腈（7:3，v/v）提取两次，经反相固相萃取（SPE）柱稀释和净化。喹诺酮类药物在反相C18柱（Hypersil BDS-C18）上分离，采用流动相梯度洗脱（乙腈和水为流动相），并用波长程序荧光检测器检测。喹诺酮类校准物在鸡肉中的线性范围为5 - 1200μg/L，相关系数大于0.998。在三个添加水平下，11种喹诺酮类药物在鸡肉中的回收率为56% - 119%，批内相对标准偏差（RSD）（0.4% - 16.1%）和批间RSD（1.4% - 23.0%）均可接受。11种喹诺酮类药物的检测限（LOD）和定量限（LOQ）分别为1 - 23μg/kg和4 - 40μg/kg。该方法的灵敏度满足残留分析的定量要求。
