张茂林, 冷晓晓, 杨福成, 龚进, 赵万江, 施丝. 超高效液相色谱-三重四级杆线性离子阱-质谱联用法定量测定全血中杀鼠醚[J]. 职业卫生与应急救援, 2019, 37(3): 287-290. DOI: 10.16369/j.oher.issn.1007-1326.2019.03.025
引用本文: 张茂林, 冷晓晓, 杨福成, 龚进, 赵万江, 施丝. 超高效液相色谱-三重四级杆线性离子阱-质谱联用法定量测定全血中杀鼠醚[J]. 职业卫生与应急救援, 2019, 37(3): 287-290. DOI: 10.16369/j.oher.issn.1007-1326.2019.03.025
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ZHANG Maolin, LENG Xiaoxiao, YANG Fucheng, GONG Jin, ZHAO Wanjiang, SHI Si. Quantitative determination of coumatetralyl in whole blood with UPLC-QTRAP-MS/MS[J]. Occupational Health and Emergency Rescue, 2019, 37(3): 287-290. DOI: 10.16369/j.oher.issn.1007-1326.2019.03.025
Citation: ZHANG Maolin, LENG Xiaoxiao, YANG Fucheng, GONG Jin, ZHAO Wanjiang, SHI Si. Quantitative determination of coumatetralyl in whole blood with UPLC-QTRAP-MS/MS[J]. Occupational Health and Emergency Rescue, 2019, 37(3): 287-290. DOI: 10.16369/j.oher.issn.1007-1326.2019.03.025
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超高效液相色谱-三重四级杆线性离子阱-质谱联用法定量测定全血中杀鼠醚

Quantitative determination of coumatetralyl in whole blood with UPLC-QTRAP-MS/MS

    摘要
  • 摘要:
    目的 建立简便、灵敏、准确的全血中杀鼠醚的定量检测方法。
    方法 采用超高效液相色谱-三重四级杆线性离子阱-质谱联用法建立全血中杀鼠醚的定量检测方法。样品经乙酸乙酯萃取，以乙酸铵（5 mmol/L）和甲醇为流动相进行梯度洗脱，在C18色谱柱上进行色谱分离，质谱检测采用电喷雾负离子化模式、多反应监测及增强子离子扫描模式。
    结果 方法的检出限为3.4 ng/mL，工作曲线在10~1 200 ng/mL范围内线性良好，三个浓度水平的样品平均加标回收率为92.5%、94.3%和101.0%，血中杀鼠醚在4℃冰箱中至少可以保存7 d。
    结论 建立的全血中杀鼠醚的定量检测方法，能减少杂质干扰，具有简便、灵敏、准确的优点，可以满足血中杀鼠醚的定量检测要求。

     

    Abstract:
    Objective To establish a simply, sensitive and accurate quantitative method for determination of coumatetralyl in blood samples.
    Methods The quantitative method of UPLC-QTRAP-MS/MS for the determination of coumatetralyl was developed. Coumatetralyl was extracted from whole blood samples by liquid-liquid extraction with ethyl acetate. The samples were extracted with ethyl acetate, then gradient eluted with ammonium acetate (5 mmol/L) -methanol as mobile phase and separated on C18 column. Electrospray ionization, multiple reaction monitoring and enhanced product ion scan mode were used for mass spectrometry detection.
    Results The detection limit of the method was 3.4 ng/mL. The working curve had a good linearity in the range of 10-1 200 ng/mL. The average recoveries of the three samples with different concentrations was 92.5%, 94.3% and 101.0%, respectively. Coumatetralyl in blood could be stored for at least 7 days at 4℃.
    Conclusion The established quantitative method could reduce the interference of impurities, and had the advantages of simplicity, sensitivity and accuracy. It could meet the requirements of quantitative detection of coumatetralyl in blood.

     

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