干旱区生态环境知识资源中心(Arid): 在线固相萃取-超高效液相色谱-串联质谱法测定尿液中芬太尼及其代谢物的含量

Arid

	在线固相萃取-超高效液相色谱-串联质谱法测定尿液中芬太尼及其代谢物的含量
其他题名	Determination of Fentanyl and Its Metabolite in Urine by On-line SPE Combined with UHPLC-MS/MS
	赵清佳; 汪蓉; 徐智儒; 盛振海; 梁晨; 张玉荣
来源期刊	理化检验. B, 化学分册
ISSN	1001-4020
出版年	2021
卷号	57 期号:6 页码:1001-4020
中文摘要	建立了在线固相萃取(on-line SPE)-超高效液相色谱-串联质谱法(UHPLC-MS/MS)测定尿液中芬太尼及其代谢物去甲芬太尼的方法,并将该方法运用于大鼠尿液中芬太尼及其代谢物的检测时限研究。将尿液用pH 9.2的2 mmol·L~(-1)甲酸铵溶液稀释,离心后直接进样。采用Oasis HLB固相萃取小柱通过在线固相萃取富集净化目标物,用pH 9.2的2 mmol·L~(-1)甲酸铵溶液淋洗,以分析泵的初始流动相将目标物洗脱至Hypesil GOLD C18分析柱上,以不同体积比的含有2 mmol·L~(-1)甲酸铵和0.1%(体积分数)甲酸的甲醇溶液、含有2 mmol·L~(-1)甲酸铵和0.1%(体积分数)甲酸的水溶液的混合液为流动相进行梯度洗脱。串联质谱分析中采用电喷雾正离子源(ESI+)和选择离子监测(SRM)模式检测。将芬太尼以20mug·kg~(-1)的给药剂量对大鼠尾静脉注射后进行尿液收集,考察原体和代谢物的检测时限。结果表明:芬太尼和去甲芬太尼的质量浓度在2.0~800 ng·L~(-1)内与其峰面积呈线性关系,检出限均为0.200 ng·L~(-1),测定值的相对标准偏差(n=5)均小于15%。在大鼠尿液中芬太尼原体的检测时限为5~7d,而其代谢物去甲芬太尼的检测时限长达28d。
英文摘要	A method was established for the determination of fentanyl and its metabolite(norfentanyl)in urine by on-line SPE combined with UHPLC-MS/MS,which was applied to the study of detection window of fentanyl and its metabolite in rat urine.The urine was diluted with 2 mmol·L~(-1) ammonium formate buffer solution at pH 9.2,and the diluted sample was directly injected after centrifugation.The target compounds were enriched and purified by on-line SPE with Oasis HLB solid phase extraction column,and eluted onto the Hypesil GOLD C18 analytical column with the initial mobile phase of the analytical pump.A mixture of methanol solution containing 2 mmol·L~(-1) ammonium formate and 0.1% (phi)formic acid,and aqueous solution containing 2 mmol·L~(-1) ammonium formate and 0.1% (phi)formic acid in different ratios was used as the mobile phase for gradient elution.ESI+and the mode of selected ion monitoring(SRM)were adopted in MS/MS.Rat urine samples were collected after the tail vein injection fentanyl of rats at a dose of 20mug·kg~(-1),and the detection window of the protosome and metabolite was studied by this method.As shown by the results,linear relationships between values of peak area and mass concentration of fentanyl and norfentanyl were found in the same range of 2.00-800 ng·L~(-1),with the same detection limit(3S/N)of 0.200 ng·L~(-1).RSDs(n=5)of the determined values were all less than 15%.The detection window of protosome fentanyl in rat urine was 5-7d,while the detection window of its metabolite norfentanyl could be up to 28d.
中文关键词	超高效液相色谱-串联质谱法 ; 在线固相萃取 ; 芬太尼及其代谢物 ; 检测时限
英文关键词	UHPLC-MS/MS on-line solid phase extraction fentanyl and its metabolite detection window
类型	Article
语种	中文
国家	中国
收录类别	CSCD
WOS类目	Chemistry
CSCD记录号	CSCD:7010930
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/365153
作者单位	赵清佳, 中国医药工业研究总院;;上海市公安局物证鉴定中心, 创新药物与制药工艺国家重点实验室;;上海市现场物证重点实验室, ;;, 上海;;上海 200040;;200083, 中国.; 汪蓉, 上海市公安局物证鉴定中心, 上海市现场物证重点实验室, 上海 200083, 中国.; 盛振海, 上海市公安局物证鉴定中心, 上海市现场物证重点实验室, 上海 200083, 中国.; 梁晨, 上海市公安局物证鉴定中心, 上海市现场物证重点实验室, 上海 200083, 中国.; 张玉荣, 上海市公安局物证鉴定中心, 上海市现场物证重点实验室, 上海 200083, 中国.; 徐智儒, 中国医药工业研究总院, 创新药物与制药工艺国家重点实验室, 上海 200040, 中国.
推荐引用方式 GB/T 7714	赵清佳,汪蓉,徐智儒,等. 在线固相萃取-超高效液相色谱-串联质谱法测定尿液中芬太尼及其代谢物的含量[J],2021,57(6):1001-4020.
APA	赵清佳,汪蓉,徐智儒,盛振海,梁晨,&张玉荣.(2021).在线固相萃取-超高效液相色谱-串联质谱法测定尿液中芬太尼及其代谢物的含量.理化检验. B, 化学分册,57(6),1001-4020.
MLA	赵清佳,et al."在线固相萃取-超高效液相色谱-串联质谱法测定尿液中芬太尼及其代谢物的含量".理化检验. B, 化学分册 57.6(2021):1001-4020.