中毒患者血浆中百草枯的LC-MS/MS定量检测方法研究

Determination of paraquat in Poisoning human plasma by LC-MS/MS method

目的使用改进的高效液相串联质谱电喷雾检测法(LC-MS/MS)测定中毒患者血浆中百草枯浓度。方法以Waters公司C18反相柱(Symmetry C18 Column,4.6mm×50mm,5μm)为色谱柱,流动相为乙腈-0.5‰的七氟丁酸水溶液(含1‰甲酸),梯度洗脱。以乙腈沉淀蛋白,氯仿反提的方法提取百草枯。样品经电喷雾离子源(ESI)正离子化后,通过三重四级杆串联质谱仪,采用多反应监测(MRM)对中毒患者血中百草枯浓度进行测定。结果对于百草枯中毒患者,可实现快速定量检测,结果相对误差小,准确度高。结论该文建立的LC-MS/MS方法简单、快速、准确,可用于检测血浆中百草枯的浓度。

Objective This study aims to develop an improved high performance liquid tandem mass spectrometry electrospray ionization （LC-MS/MS） for paraquat detection in human plasma.Methods The human plasma was treated by acetonitrile precipitation to remove protein components from human plasma,and then treated by chloroform.The Supernatant was separated on a Waters C18 column with a gradient elution.The mobile phase consisted acetonitrile with 0.5‰ heptafluorobutyric acid solution （containing 1‰ formic acid）.Samples were ionized by triple quadrupole tandem mass spectrometer and measured using multiple reaction monitoring （MRM） of paraquat.Single point external standard method was adopted as the quantitative methods to shorten the test time.Results This method was applied to determine the paraquat concentration in the blood of patients with paraquat poisoning.The measurement results were used to evaluate severity of these patients and predict the prognosis of patients,which can help to select rational treatments for patients.Conclusion It is a rapid,sensitive,accurate and reliable method for the determination of paraquat concentration in the blood of poisoned patients.