摘要
目的 建立血液、胃液中地芬尼多的高效液相色谱-时间飞行质谱快速测定方法。方法 样品经乙腈沉淀蛋白,高速离心,上清液经色谱柱分离,电喷雾正离子模式进行检测,用标准加入法定量分析。结果 血液、胃液等样品经前处理后,用乙腈、0.1%甲酸水溶液做流动相,用EC-C18做色谱柱时,地芬尼多与样品中的杂质有较好的分离,实验可在120 min内完成,与标准图谱进行检索匹配结合保留时间匹配可得到准确可靠的定性分析结果;血清样品以地芬尼多的母离子m/z 310.216 5为定量离子,地芬尼多浓度与定量离子峰面积有良好线性关系,线性范围为0μg/L~160μg/L,线性系数为0.999 8,检出限为0.9μg/L,加标回收率为96.0%~114.1%,相对标准偏差为1.33%~4.15%。结论 该方法具有前处理简单、检测速度快、灵敏度高、干扰少等优点,适用于血液、胃液中的地芬尼多的快速定性定量测定。
Objective This paper aims to establish a high performance liquid chromatography-time flight mass spectrometry method for the detection of difenidol in blood and gastric juice.Methods The samples were precipitated by acetonitrile and centrifuged at high speed.The supernatant was separated by chromatographic column.The electrospray positive ion mode was used for detection and quantitative analysis by standard addition method.Results When acetonitrile and 0.1%formic acid aqueous solution were used as mobile phase and EC-C18 was used as chromatographic column,diphenidol was well separated from impurities in the samples after pretreatment.The experiment could be completed within 120 min,and accurate and reliable qualitative analysis results could be obtained by searching and matching with standard chromatogram and retention time matching.The concentration of diphenidol had a good linear relationship with the peak area of diphenidol,with parent ions m/z 310.2165 of diphenil as the quantitative ion.The linear range was 0μg/L-160μg/L,the linear coefficient was 0.9998,the detection limit was 0.9μg/L,and the recoveries were 96.0%-114.1%.The relative standard deviation(RSD)was 1.33%-4.15%.Conclusion The method has the advantages of simple pretreatment,fast detection speed,high sensitivity and less interference,and is suitable for the rapid qualitative and quantitative determination of difenidol in blood and gastric juice.
作者
陈纠
郭冠浩
郭嘉明
周丽屏
王致
CHEN Jiu;GUO Guan-hao;GUO Jia-ming;ZHOU Li-ping;WANG Zhi(Guangzhou Occupational Disease Prevention Hospital,Guangdong 510620,China)
出处
《中国卫生检验杂志》
CAS
2023年第9期1046-1048,1066,共4页
Chinese Journal of Health Laboratory Technology
基金
广州市高水平临床重点专科建设项目(穗卫函[2019]1555号)
广州市医学重点学科建设项目(2021-2023)
广州市科学技术局重点研发计划项目(2022060-10061)。
关键词
血液
胃液
地芬尼多
高效液相色谱-飞行时间质谱法
Blood
Gastric juice
Difenidol
High performance liquid chromatography-time of flight mass spectrometry
