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目的建立血浆中氟吡酰草胺的气相色谱-质谱测定方法。方法血浆中的氟吡酰草胺经乙腈提取,DB-5MS毛细管气相色谱柱分离,采用气相色谱-质谱联用仪检测,选择离子模式,定性离子质荷比(m/z)376,定量离子m/z 238。结果血浆中氟吡酰草胺在质量浓度为10.00~1 200.00μg/L范围内线性关系良好,相关系数为0.999 4,检出限为2.5μg/L,定量下限为7.5μg/L(取血浆0.20 m L)。批内相对标准偏差(RSD)为0.39%~6.52%,批间RSD为0.93%~8.80%,加标回收率为95.25%~99.48%,样品在-18℃条件下至少可以保存10 d。结论本方法灵敏度高、精密度和准确度好、操作简便,可作为氟吡酰草胺代谢研究中血浆中氟吡酰草胺水平的检测方法。
Objective To establish a method for the determination of picifamide in plasma by gas chromatography-mass spectrometry. Methods The plasma of picolimit was extracted with acetonitrile and separated on a DB-5MS capillary gas chromatographic column. Gas chromatography-mass spectrometry (GC-MS) m / z 238. Results The linear range of the concentration of picolofos in the range of 10.00-1 200.00 μg / L was good, the correlation coefficient was 0.999 4, the detection limit was 2.5 μg / L and the lower limit of quantitation was 7.5 μg / L 0.20 m L). The relative standard deviations (RSDs) were 0.39% ~ 6.52%. The RSDs between batches were 0.93% ~ 8.80%. The recoveries were 95.25% ~ 99.48%. The samples were stored at -18 ℃ for at least 10 days. Conclusion The method has high sensitivity, good precision and accuracy, and is easy to operate. It can be used as a detection method for the level of picolimid in the metabolism of picolimil.