鸡蛋中环丙沙星、恩诺沙星残留物HPLC-MS/MS分析

Determination of Ciprofloxacin and Enrofloxacin Residues in Eggs by HPLC-MS/MS

目的建立鸡蛋中环丙沙星、恩诺沙星残留物液相色谱-串联质谱(LC-MS/MS)检测方法。方法鸡蛋中环丙沙星、恩诺沙星用酸性乙腈提取,正己烷除脂,采用Waters ACQUITY UPLC?BEH C18色谱柱(2.1mm×100mm,1.7μm)分离,电喷雾离子源在正离子模式下电离,多反应监测(MRM)模式扫描。结果环丙沙星和恩诺沙星分别在5.194～129.85 ng/ml和2.154～53.85 ng/ml范围内线性关系良好,线性方程分别为Y=1300X+17.7(r=0.9999)、Y=1450X-658(r=0.9993)。环丙沙星和恩诺沙星定量限(S/N=10)分别为1.0388μg/kg和0.4308μg/kg。分别添加环丙沙星含量为1.0388,2.597μg/kg,恩诺沙星含量为0.4308,1.077μg/kg的对照品溶液于阴性鸡蛋基质中,回收率分别90.7%～107.6%、80.1%～101.6%和85.0%～105.4%、86.9%～103.6%。结论该方法简单、灵敏、准确,可以作为鸡蛋中环丙沙星、恩诺沙星的检测方法之一。

Objective To establish a method for the determination of ciprofloxacin and enrofloxacin residues in eggs by liquid chromatography-tandem mass spectrometry （LC-MS/MS）. Methods The ciprofloxacin and enrofloxacin residues in eggs were extracted by acidic acetonitrile frst, then the lipid substances were removed by hexane. The samples were separated by Waters ACQUITY UPLC BEH C18 column （2.1 mm×100 mm, 1.7 μm）. The analysis was performed by MS/MS with electrospray ionization in positive ion mode with multiple reaction monitoring （MRM）.Results Ciprofloxacin and enrofloxacin showed a good linearity at the range of 5.194-129.85 ng/ml and 2.154-53.85 ng/ml, respectively, with the linear equation Y=1300X＋17.7, r=0.9999 for ciprofloxacin, Y=1450X-658, r=0.9993 for enrofloxacin. The quantifcation limit of ciprofloxacin was 1.0388 μg/kg, and that of enrofloxacin was 0.4308 μg/kg. The recoveries were 90.7 %-107.6 %, 80.1 %-101.6 %, 85.0 %-105.4 %, 86.9 %-103.6 % respectively at two content adding levels of ciprofloxacin and enrofloxacin, namely 1.0388 μg/kg, 2.597 μg/kg for ciprofloxacin, 0.4308 μg/kg, 1.077 μg/kg for enrofloxacin. Conclusion This method has the advantages of simple pretreatment, sensitivity and accuracy and it can be regarded as the technique of determination of ciprofloxacin and enrofloxacin in egg.