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固相萃取-高效液相色谱法对血液中唑吡坦及其两种羧酸代谢物的同时测定
其他题名Simultaneous Determination of Zolpidem and Its Two Carboxyl Metabolites in Blood by High Performance Liquid Chromatography with Solid Phase Extraction
朱定姬1; 黄克建2; 林翠梧1; 李宏森2; 刘晓锋2; 李璐2; 陈而廉3
来源期刊分析测试学报
ISSN1004-4957
出版年2010
卷号29期号:1页码:22-25
中文摘要建立了固相萃取-高效液相色谱分析血液中唑吡坦、6-羧酸唑吡坦及苯基-4-羧酸唑吡坦的方法.采用Waters Oasis~(R) HLB 3 mL固相萃取小柱萃取,以乙腈-2.5 mmol/L醋酸铵水溶液为流动相,梯度洗脱,经ZORBAX Eclipse XDB-C_(18)色谱柱(4.6 mm*250 mm,5 mum)分离,二极管阵列检测器(DAD)检测,检测波长为250 nm,外标法定量.比较了不同洗脱溶剂、溶液pH值对回收率的影响.在优化条件下,唑吡坦、6-羧酸唑吡坦及苯基-4-羧酸唑吡坦的线性范围分别为40 ~2 000 mug/L(r=0.999 9)、20 ~2 000 mug/L(r=0.999 8)和40 ~2 000 mug/L(r=0.999 8),检出限为1.2 ~3.3 mug/L.添加16、160、360 mug/L 3个水平的混合标准溶液,3种化合物的回收率为86% ~106%,相对标准偏差均小于8%.结果表明,该方法具有操作简便、回收率高、精密度好和灵敏度高等特点,适于血液中唑吡坦及其2个羧酸代谢物的分析,可为相关案件提供方法及技术支持.
英文摘要A solid phase extraction-high performance liquid chromatographic method was developed for analysis of zolpidem,zolpidem 6-carboxylic acid(ZCA) and zolpidem phenyl-4-carboxylic acid(ZPCA) in blood sample.The sample was extracted by Waters Oasis~(R) HLB 3 mL solid phase column and separated on an ZORBAX Eclipse XDB-C_(18) column(4.6 mm*250 mm,5 mum) under gradient condition using acetonitrile and 2.5 mmol/L ammonium acetate water solution as the mobile phase.Analysis of zolpidem,ZCA and ZPCA were performed by photo diode array detection(DAD) at 250 nm with external standard method.The eluting solvent and pH value of solution on the recoveries were investigated and the chromatogramic conditions were optimized.Under the optimal condition,the method showed good linearity in the ranges of 40-2 000 mug/L for zolpidem(r=0.999 9),20-2 000 mug/L for ZCA(r=0.999 8),and 40-2 000 mug/L for ZPCA(r=0.999 8).The limits of detection were between 1.2 and 3.3 mug/L.The recoveries of zolpidem and two carboxyl metabolites were from 86% to 106% at three spiked levels of 16,160 and 360 mug/L.The relative standard de- viations(RSDs) of the method were less than 8%.The results indicated that this method was simple,accurate and sensitive,and was suitable for the analysis of zolpidem and its two carboxyl metabolites in the blood sample.
中文关键词高效液相色谱法 ; 固相萃取 ; 唑吡坦 ; 羧酸代谢物 ; 血液
英文关键词high performance liquid chromatography(HPLC) solid phase extraction zolpidem carboxyl metabolites blood
语种中文
国家中国
收录类别CSCD
WOS类目CHEMISTRY ANALYTICAL ; PHARMACOLOGY PHARMACY
WOS研究方向Chemistry ; Pharmacology & Pharmacy
CSCD记录号CSCD:3811047
资源类型期刊论文
条目标识符http://119.78.100.177/qdio/handle/2XILL650/224908
作者单位1.广西大学化学化工学院, 南宁, 广西 530004, 中国;
2.广西壮族自治区公安厅,物证鉴定中心, 南宁, 广西 530012, 中国;
3.广西壮族自治区公安厅,科技处, 南宁, 广西 530012, 中国
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GB/T 7714
朱定姬,黄克建,林翠梧,等. 固相萃取-高效液相色谱法对血液中唑吡坦及其两种羧酸代谢物的同时测定[J],2010,29(1):22-25.
APA 朱定姬.,黄克建.,林翠梧.,李宏森.,刘晓锋.,...&陈而廉.(2010).固相萃取-高效液相色谱法对血液中唑吡坦及其两种羧酸代谢物的同时测定.分析测试学报,29(1),22-25.
MLA 朱定姬,et al."固相萃取-高效液相色谱法对血液中唑吡坦及其两种羧酸代谢物的同时测定".分析测试学报 29.1(2010):22-25.
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