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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
孙雷
0
(中国兽医药品监察所)
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%。
关键词:  氟喹诺酮类药物  猪肉  高效液相色谱-串联质谱
DOI:
投稿时间:2008-01-04修订日期:2008-01-04
基金项目:
Determination of Fluoroquinolones in Pig Muscle by HPLC-MS/MS
Sun Lei
()
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%.
Key words:  Fluoroquinolones  pig muscle  HPLC-MS/MS

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