硫酸博来霉素中组胺残留方法学研究

The residual research method of histamine in bleomycin sulfate

目的建立硫酸博来霉素中组胺残留研究方法。方法采用Agilent Eclipse Plus C_(18)(3.0mm×100mm,1.8μm)色谱柱,流动相A为0.01mol/L乙酸铵(甲酸调pH至3.0),流动相B为乙腈,梯度洗脱,质谱检测器,流速0.3mL/min。结果组胺的线性范围为1.02~50.81ng/mL,相关系数r>0.99,方法检出限浓度为0.30ng/mL(相当于样品浓度0.38ppm),定量限浓度为1.02ng/mL(相当于样品浓度1.28ppm),样品加标回收率在80%~120%。结论该方法无需衍生,可以快速、简便、灵敏、准确地用质谱来定性定量测定硫酸博来霉素中组胺含量。

Objective To establish a residual research method of histamine in bleomycin sulfate.Methods An Agilent Eclipse Plus C_(18)(3.0 mm×100 mm,1.8μm)column as used.The mobile phase consisted of 0.01 mol/L ammonium acetate(pH3.0)was used as the mobile phase A and acetonitrile as the mobile phase B.Gradient elution was used.The detector was the mass spectrometer.The flow rate was 0.3 mL/min.Results The linear range was 1.02~50.81 ng/mL with the correlation coefficients above 0.99.The limit of detection was 0.30 ng/mL(equivalent to 0.38 ppm of sample concentration),the limit of quantification was 1.0 ng/mL(equivalent to 1.28 ppm of sample concentration),and the recoveries were between 80%~120%.Conclusion The method is rapid,simple,sensitive,and accurate for the qualitative and quantitative determination of histamine without derivatization in bleomycin sulfate.