HPLC-MS/MS同时定量检测血浆中多种农药浓度及临床意义  

Simultaneous Quantitative Detection of Multiple Pesticides in Human Plasma by HPLC-MS/MS and Clinical Significance of the Results

作　　者：林淑瑜 戴立 邓卫东 许琨琨 LIN Shu-yu;DAI Li;DENG Wei-dong;XU Kun-kun(Dept.of Pharmacy,No.910 Hospital of PLA,Quanzhou 362000,China;Quanzhou Food and Drug Inspection Institute,Quanzhou 362018,China)

机构地区：[1]中国人民解放军联勤保障部队第910医院药剂科,福建泉州362000 [2]泉州市食品药品检验所,福建泉州362018

出　　处：《海峡药学》2022年第11期75-79,共5页Strait Pharmaceutical Journal

基　　金：泉州科技计划项目(2018Z146)。

摘　　要：目的 建立高效液相色谱串联质谱(HPLC-MS/MS)法同时测定人血浆中11种农药(乐果、氧乐果、敌敌畏、毒死蜱、辛硫磷、丙溴磷、三唑磷、甲基硫菌灵、稻瘟灵、溴鼠隆、阿维菌素)含量的方法及分析中毒物检测的临床意义。方法 新鲜血样离心后得到的血浆用4℃~8℃冷藏的75%乙腈沉淀蛋白,再用高效液相色谱-串联质谱法(HPLC-MS/MS)进行测定,色谱柱采用ACQUITY UPLC C_(18)(2.1×50 mm, 1.7μm),流动相为0.1%甲酸水溶液-乙腈,梯度洗脱,采用正离子多反应监测(MRM)模式检测。结果 血样中11种农药的线性范围为2~100 ng·mL^(-1),相关系数(r)>0.9952,血样的最低检测限<0.5 ng·mL^(-1)。添加标样浓度水平为10 ng·mL^(-1)、50 ng·mL^(-1)、100 ng·mL^(-1)时,回收率为64.34%~106.81%;低、高2种浓度水平的日内、日间相对标准偏差(RSD)小于10%。结论 本方法检测方便快捷,检测限低,准确性好,可在短时间内给出定性、定量分析结果,可用于临床中毒患者的血浆中毒物的检测,指导临床抢救治疗。OBJECTIVE To establish a method for the determinations of 11 pesticides in plasma simultaneously, including dimethoate, omethoate, dichlorvos, chlorpyrifos, phoxim, profenofos, triazophos, thiophanate-methyl, rice blast spirit, bromopyrone, abamectin, and analysis the clinical significance of the results.METHODS The plasma samples from the fresh blood samples after centrifugation were analyzed by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) after being purified by protein precipitation with 75% acetonitrile stored under refrigeration(4 ℃-8 ℃).The quantitative analysis was performed on ACQUITY UPLC C_(18)(2.1× 50 mm, 1.7 μm),with a mobile phase of 0.1% formic acid solution-acetonitrile with gradient elution in multiple reaction monitoring(MRM) mode via positive electrospray ionization.RESULTS The linear range of 11 pesticides was among 2-100 ng·mL,and the correlate coefficient(r) was greater than 0.9952,with the lowest quantification concentration<0.5 ng·mL^(-1).And at the spiked levels of 10 ng·mL^(-1)、50 ng·mL^(-1)、100 ng·mL^(-1),the recovery rates were among 64.34%-106.81%,and the intra-day relative standard deviations(RSD) at low and high concentrations were less than 10%.CONCLUSION The detection method is convenient and quick, with low detection limit and good accuracy, and can acquire the analysis results of qualitative and quantitative in a short time, which can be used for the detection of plasma toxicants in clinical poisoning patients and guide clinical rescue treatment.

关 键 词：HPLC-MS/MS 农药中毒 血药浓度 血浆 

分 类 号：R969.1[医药卫生—药理学]