摘要
目的 :建立检测生物样本(全血、尿液、唾液)中所含巴比妥、苯巴比妥、异戊巴比妥药物成分的QuEChERS-超高效液相色谱(UPLC)-多重反应监测(MRM)-条件触发(IDA Criteria)-增强子离子扫描(EPI)检测方法。方法 :色谱柱为Waters Atlantis T3 C_(18),100 mm×2.1 mm,3μm;柱温为40℃;流动相为含0.1%甲酸的5 mmol/L甲酸铵水溶液及乙腈,梯度洗脱15 min;流速为0.2 mL/min;以优化后的质谱参数采集信号。结果 :检出限浓度为0.5 ng/mL;定量限浓度为1.0 ng/mL;线性范围为定量限浓度～200 ng/mL;在线性范围内相关系数在0.999以上;加标回收率为88.0%～96.8%。结论 :本方法准确,灵敏度高,专属性好;能用于生物样本(全血、尿液、唾液)中巴比妥、苯巴比妥、异戊巴比妥化学成分的同时定性及定量检测。
Objective: To establish a QuEChERS-ultrahigh performance liquid chromatography (UPLC)-multiple reaction monitoring (MRM)-conditional trigger (IDA Criteria)-enhanced product ion scan (EPI) method for the determination of barbital, phenobarbital and amobarbital in biological samples (whole blood, urine, saliva). Method: The chromatographic column was Waters Atlantis T3 C18, 100 mm × 2.1 mm, 3 μm;the column temperature was 40℃;the mobile phase was 5 mmol/L ammonium formate aqueous solution containing 0.1% formic acid and acetonitrile for gradient elution at 0.2 mL/min for 15 min;the signal was acquired with optimized mass spectrometry parameters. Results: The detection limit was 0.5 ng/mL;the limit of quantitation was 1.0 ng/mL;the linear range was 1.0 ng/mL^200 ng/mL;the correlation coefficient within the linear range was above 0.999;the recoveries of addition standard were 88.0%~96.8%. Conclusion: This method is accurate, sensitive and specific. It can be used for simultaneous qualitative and quantitative detection of barbital, phenobarbital and amobarbital in biological samples (whole blood, urine, saliva).
作者
涂凤莲
熊周芳
汪元符
Tu Feng-lian;Xiong Zhou-fang;Wang Yuan-fu(Xinjian District Hospital of Traditional Chinese Medicine,Jiaingxi Nanchang 330100,China;Nanchang Institute for Food and Drug Control,Jiangxi Nanchang 330038,China)
出处
《中国执业药师》
CAS
2018年第11期145-149,155,共6页
China Licensed Pharmacist
基金
南昌市指导性科技计划项目(洪科发计字【2016】96号)
