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    超高效液相色谱-串联质谱法测定豆芽中恩诺沙星和环丙沙星

    UHPLC-MS/MS Determination of Enrofloxacin and Ciprofloxacin in Bean Sprouts

    • 摘要: 匀浆混匀的豆芽样品经磷酸盐缓冲溶液超声提取,提取液经HLB固相萃取小柱净化,甲醇洗脱。采用超高效液相色谱-串联质谱法测定恩诺沙星和环丙沙星的含量,以Agilent Eclipse Plus C18 RRHD色谱柱为固定相,以不同体积比的甲醇和0.1%(体积分数)甲酸-2 mmol·L-1乙酸铵溶液的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾正离子源和多反应监测模式。采用同位素内标法定量,恩诺沙星和环丙沙星的线性范围均为0.5~50.0 μg·L-1,检出限(3S/N)均为0.025 μg·kg-1。以空白样品为基体进行加标回收试验,所得回收率为89.2%~101%,测定值的相对标准偏差(n=6)为3.3%~9.2%。

       

      Abstract: The bean sprout sample blended with homogenizer was extracted ultrasonically with phosphate buffer. The extract was purified with HLB solid phase extraction column, and then eluted with methanol. UHPLC-MS/MS was applied to the determination of enrofloxacin and ciprofloxacin. Agilent Eclipse Plus C18 RRHD chromatographic column was used as stationary phase, and the mixture of methanol and 0.1% (φ) formic acid-2 mmol·L-1 ammonium acetate solution mixed in different ratios was used as mobile phase in gradient elution. ESI+ and multi-reactions monitor mode were adopted in MS/MS. Isotope was used as internal standard. Linearity ranges of enrofloxacin and ciprofloxacin were both found between 0.5 μg·L-1 and 50.0 μg·L-1, with detection limit (3S/N) of 0.025 μg·kg-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 89.2%-101%, with RSDs (n=6) of determined values in the range of 3.3%-9.2%.

       

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