猪肉组织中7种氟喹诺酮类药物残留检测高效液相色谱-串联质谱法研究

Determination of Fluoroquinolones in Pig Muscle by HPLC-MS/MS

关键词:  氟喹诺酮类药物  猪肉  高效液相色谱-串联质谱

Key words:  Fluoroquinolones  pig muscle  HPLC-MS/MS

摘要:

建立了猪肉组织中氧氟沙星、诺氟沙星、环丙沙星、恩诺沙星、达氟沙星、二氟沙星和沙拉沙星7种氟喹诺酮类药物残留检测的高效液相色谱-串联质谱方法。液相色谱条件为：色谱柱为XBridge C18柱（150×2.1mm,5µm）；流动相为0.1％甲酸甲醇溶液＋0.1％甲酸水溶液，梯度洗脱；柱温为30℃；流速为0.2mL/min；进样量为20µL。质谱条件为：电喷雾离子源（ESI＋），多反应监测（MRM）方式采集。以诺氟沙星-D5作内标，内标法定量。结果表明：7种FQs药物在5～250ng/mL浓度范围内呈现良好线性关系，相关系数R2均大于0.997；方法检测限为5ng/g，定量限为10ng/g；从10、20和100ng/g三个添加浓度检测结果可以看出，方法平均回收率为80.7%～116%（n＝6），批内批间RSD均小于20％。

Abstract:

A HPLC-MS/MS method was established for the determination of Ofloxacin, Norfloxacin,Ciprofloxacin, Enrofloxacin, Danofloxacin, Difloxacin and Sarafloxacin in pig muscle. HPLC condition: the chromatography column is XBridge C18 column of 150×2.1mm,5µm；mobile phase is methanol(0.1% formic acid) and water(0.1% formic acid)；column temperature is 30℃；flow rate is 0.2 mL/min；injection volume is 20µL. Mass Spectrometry condition: ESI+ and MRM mode. The calibration curve was good linear between the ratio of the peak areas and concentrations of Fluoroquinolones from 5 to 250 ng/mL containing the internal standard at 20 ng/mL，the correlation coefficient R2＞0.997. The limit of detection of the method was 5ng/g, and the limit of quantification was 10ng/g. The average recoveries from spiked pig muscle at the three concentrations of 10,20 and 100ng/g ranged from 80.7%～116%（n＝6）, and intra- and inter-batch variation coefficients were less than 20%.