目的建立环境水样中诺氟沙星的电喷雾萃取电离质谱(EESI-MS)快速测定法。方法将经过简单过滤后的环境水样直接进行电喷雾萃取电离质谱分析,雾化气压力为1.6 MPa,质谱离子传输管温度为200℃,喷雾电压为2.5 k V;以甲醇溶液为喷雾溶剂,流速为4μl/min;样品溶液流速为11μl/min。结果在50-10 000μg/L的线性范围内,该方法的线性回归方程为y=0.875 8x-0.289,r=0.999 8。该方法的检出限为1.53μg/L,加标回收率为76.2%-86.5%,RSD为1.12%-8.55%。结论该方法灵敏度高、精密度好、分析速度快、能够承受环境水样中复杂基体的影响,适用于环境水样中诺氟沙星的直接定量检测。
Objective To develop a rapid and sensitive extractive electrospray ionization mass spectrometry(EESI-MS) method for the determination of norfloxacin in environmental water samples. Methods The environmental water samples with simple filtering were directly analyzed by EESI-MS and the pressure of atomizing air,temperature of ion transport,electrospray voltage were 1.6 MPa,200 ℃,2.5 k V,respectively. The CH3 OH was used as electrospray solvent with 4 μl/min flow rate and the sample flow rate was 11 μl/min. Results Under the optimized working conditions,the calibration graph was linear in the range of 50-10 000 μg/L(r=0.999 8). The limit of detection was 1.53 μg/L. The relative standard deviations were ranged from 0.54%to 6.93% and the recovery rates were 76.2%-86.5%. Conclusion The results show that EESI-MS is a powerful analytical platform to provide high sensitivity,high precision,rapid analysis and high specificity for quantitative analysis of norfloxacin in environmental water samples.