共查询到20条相似文献,搜索用时 62 毫秒
1.
目的:建立大鼠血浆中灯盏乙素的RP-HPLC测定法.方法:RP-HPLC法,采用迪马C18柱(250 mm×4.6 mm,5 μm),甲醇-乙腈-0.01 mol/L乙酸铵溶液(pH 3.5)(22:8:70)为流动相,流速为1.0 ml/min,检测波长335 nm,柱温30 ℃.结果:线性范围为0.025~20.0 mg/L(r=0.999 9),最低定量浓度为25 ng/ml.结论:建立的大鼠血浆中灯盏乙素的反相液相色谱测定法灵敏、准确,可用于大鼠血浆中灯盏乙素浓度测定. 相似文献
2.
灯盏细辛注射液55例不良反应分析 总被引:4,自引:0,他引:4
通过文献检索.查阅1997年1月-2005年6月国内公开发行的中文医药期刊,对有关灯盏细辛注射液的ADR进行分类统计分析。结果灯盏细辛注射液所致的ADR报道共55例,ADR中无性别选择性,30岁以上为多发人群。ADR类型中变态反应占42.98%.轻者发生皮疹.重者可发生过敏性休克。 相似文献
3.
4.
注射用灯盏花素治疗脑梗塞106例的疗效验证观察 总被引:3,自引:1,他引:2
自1994年8月~1995年3月我省临床应用注射用灯盏花素(冻干粉针剂),取得了较好的效果,现报告如下。临床资料 病例选择 本组病例均为住院患者,经临床、CT、MRI检查确诊为脑梗塞的患者。采用单盲对照,随机选择发病在1月内的病例分为3组:A组为注谢用灯盏花素治疗组106例,男55例,女51例,年龄44~82岁,平均63-41±12-68岁。B组为云南灯盏花注射液对照组50例,男22例,女28例,年龄52~79岁,平均65-5±10-25岁。C组为复方丹参对照组44例,男26例,女18例,年龄4… 相似文献
5.
6.
灯盏花素的临床应用极其广泛,近年来其药动学研究也日趋活跃。本文从研究方法、吸收、分布、代谢、排泄等方面综述灯盏花素的药动学研究进展,为今后的研究提供理论基础。 相似文献
7.
灯盏乙素的药物动力学研究现状 总被引:3,自引:0,他引:3
综述灯盏乙素在药物动力学中研究对象、给药剂型与途径、研究方法(分为血药浓度法、尿药排泄数据法、药理效应法,其中血药浓度法最为常用)、吸收、分布、消除、生物转化和总体水平模型等方面的研究进展。 相似文献
8.
9.
10.
11.
12.
LC/MS/MS的多反应监测方法定量测定灯盏乙素 总被引:14,自引:2,他引:12
目的:建立一种可靠的灯盏乙素定量分析方法。方法:用三级四极串联质谱(MS/MS)作为HPLC的检测器,其中MS/MS使用了多反应监测(MRM)扫描方式。选择母→子离子对m/z -461→m/z -285作为MRM监测的离子对;HPLC流动相为100%甲醇,流速0.9 mL.min-1,色谱柱Beckman ODS-1。以测定短葶飞蓬提取物的灯盏乙素含量为例,对此方法进行了应用。结果:灯盏乙素在短葶飞蓬提取物中含量为6.98%。方法线性范围20~160 ng.mL-1 (γ=0.999);加入灯盏乙素标准品20,60和160 ng的加样回收率分别为:96.5%,97.4%和97.3%。检测限为1 ng,每个样品的分析时间为4 min。结论:此法灵敏、快速、准确,可应用于灯盏乙素的各种药剂、药代的研究。 相似文献
13.
14.
Determination of a selection of synthetic cannabinoids and metabolites in urine by UHPSFC‐MS/MS and by UHPLC‐MS/MS
下载免费PDF全文
![点击此处可从《Drug testing and analysis》网站下载免费的PDF全文](/ch/ext_images/free.gif)
Thomas Berg Lakhwinder Kaur Anna Risnes Stine Marie Havig Ritva Karinen 《Drug testing and analysis》2016,8(7):708-722
Two different analytical techniques, ultra‐high performance supercritical fluid chromatography‐tandem mass spectrometry (UHPSFC‐MS/MS) and reversed phase ultra‐high performance liquid chromatography‐tandem mass spectrometry (UHPLC‐MS/MS), were used for the determination of two synthetic cannabinoids and eleven metabolites in urine; AM‐2201 N‐4‐OH‐pentyl, AM‐2233, JWH‐018 N‐5‐OH‐pentyl, JWH‐018 N‐pentanoic acid, JWH‐073 N‐4‐OH‐butyl, JWH‐073 N‐butanoic acid, JWH‐122 N‐5‐OH‐pentyl, MAM‐2201, MAM‐2201 N‐4‐OH‐pentyl, RCS‐4 N‐5‐OH‐pentyl, UR‐144 degradant N‐pentanoic acid, UR‐144 N‐4‐OH‐pentyl, and UR‐144 N‐pentanoic acid. Sample preparation included a liquid‐liquid extraction after deconjugation with ß‐glucuronidase. The UHPSFC‐MS/MS method used an Acquity UPC2 TM BEH column with a mobile phase consisting of CO2 and 0.3% ammonia in methanol, while the UHPLC‐MS/MS method used an Acquity UPLC® BEH C18 column with a mobile phase consisting of 5 mM ammonium formate (pH 10.2) and methanol. MS/MS detection was performed with positive electrospray ionization and two multiple reaction monitoring transitions. Deuterated internal standards were used for six of the compounds. Limits of quantification (LOQs) were between 0.04 and 0.4 µg/L. Between‐day relative standard deviations at concentrations ≥ LOQ were ≤20%, with biases within ±19%. Recoveries ranged from 40 to 90%. Corrected matrix effects were within 100 ± 10%, except for MAM‐2201 with UHPSFC‐MS/MS, and for UR‐144 N‐pentanoic acid and MAM‐2201 N‐4‐OH‐pentyl with UHPLC‐MS/MS. Elution order obtained by UHPSFC‐MS/MS was almost opposite to that obtained by UHPLC‐MS/MS, making this instrument setup an interesting combination for screening and confirmation analyses in forensic cases. The UHPLC‐MS/MS method has, since August 2014, been successfully used for confirmation of synthetic cannabinoids in urine samples revealing a positive immunoassay screening result. Copyright © 2015 John Wiley & Sons, Ltd. 相似文献
15.
16.
HPLC/MS/MS联用技术测定全血中的瑞芬太尼 总被引:2,自引:1,他引:2
目的:建立全血中瑞芬太尼的HPLC/MS/MS测定方法,并测定围麻醉期患者体内瑞芬太尼的血药浓度。方法:全血样品中加入枸橼酸芬太尼作内标,用1-氯丁烷进行提取。以乙腈与三氯甲烷(V乙腈:V三氧甲烷= 1:1)混合液加乙酸铵(2 mmol·L-1)为流动相,色谱柱为Intersil ODS-3(50 mm×2.1 mm,3μm),流速0.3 mL·min-1。三级四极杆质谱采用正离子模式,离子采集方式为多反应监测模式(MRM),离子源温度200℃,离子源电离电压为5 000 V,雾化气流速8 L·min-1。采集离子(母离子/子离子)为瑞芬太尼377/228,芬太尼337/188。结果:瑞芬太尼在0.5~50.0 ng·mL-1浓度范围内呈良好的线性(r=0.9994)。日内、日间精密度均在15%以内,提取回收率大于67.3%,方法回收率在95.0%~97.6%。结论:本方法灵敏、准确,适合瑞芬太尼的体内分析。 相似文献
17.
System suitability is widely recognized as a critical component of bioanalysis. This paper discusses a generic system suitability test that monitors instrument performance throughout a run when used for liquid chromatography tandem mass spectrometry (LC/MS/MS) in bioanalysis. This system suitability process is designed to ensure that the LC/MS/MS system is performing in a manner that leads to the production of accurate and reproducible data that can be submitted with confidence to regulatory agencies. This process contains tests for signal stability, carryover, and instrument response. This approach is integrated throughout an analytical run and has been used in the analysis of over 25,000 batches of clinical samples. Two case studies are presented in which quality control samples and standards meet all acceptance criteria (based on Standard Operating Procedures and the Food and Drug Administration's recommendations for bioanalytical method validation) but failed the proposed system suitability test, and thus were rejected. In these case studies, the concentrations of a significant number of clinical samples (over 35%) were affected, resulting in changes of more than 15% when the samples were reanalyzed. These data indicate that the poor performance of an LC/MS/MS system could adversely affect the calculated concentrations of unknown samples even though the results for quality control samples appear to be acceptable. 相似文献
18.
液相色谱-质谱联用法测定人血浆双氢青蒿素浓度 总被引:2,自引:0,他引:2
目的:建立液相色谱-质谱联用法测定健康人血浆中双氢青蒿素浓度的方法。方法:以青蒿素为内标,血浆样品采用液-液萃取法处理。用电喷雾离子化和正离子多离子反应监测方式检测双氢青蒿素。结果:该方法双氢青蒿素线性范围为1.01~2020 ng.ml-1;定量下限为1.001±0.072 ng.ml-1;方法回收率在93.0%~98.2%;批内、批间变异系数均<10%。结论:该方法准确、灵敏、特异、简便,适用于健康人血浆双氢青蒿素浓度的测定。 相似文献
19.
UPLC(超高效液相色谱)/MS/MS联用技术测定全血中的西罗莫司 总被引:2,自引:0,他引:2
目的 建立全血中西罗莫司的UPLC(超高效液相色谱)/MS/MS测定方法,方法 全血样品中加入他克莫司(FK506)作内标,用叔丁基甲醚进行提取。以乙腈与含千分之五甲酸的水溶液为流动相(40:50),色谱柱为AcquityUPLCTMBEHC。(50mm×2.1mm,1.7μm),流速0.5ml/min。三重四极杆质谱采用正离子模式,离子采集方式为多反应监测模式(MRM),离子源温度105℃,离子源电离电压为3300V,雾化气流速500L/h。采集离子(母离子/子离子)西罗莫司为931.2/864.1,FK506为822.0/577.0。结果 西罗莫司在1~240腿/L浓度范围内呈良好的线性(n=0.9995)。日内、日间精密度均在15%以内,提取回收率大于75.0%,方法回收率为95.0%~98.5%,最低检测限为0.2μg/L。结论 本方法灵敏、准确,适合临床西罗莫司的全血分析。 相似文献
20.
目的建立测定人血浆中氯吡格雷(抗心肌及抗脑梗死药)血药浓度的HPLC/MS/MS法。方法血浆样品用叔丁基甲醚提取,内标为噻氯匹定;色谱柱用X-Terra MS C_(18)(2.1 mm×50 mm,5μm),柱温30℃,流动相:乙腈-水(含10 mmol·L~(-1)醋酸铵,调pH为4.0)为70:30,流量为0.3 mL·min~(-1);质谱用ESI离子源,定量分析的离子反应分别为m/z 322→z 212 (氯吡格雷),m/z 264→m/z 154(内标噻氯匹定)。结果氯吡格雷的线性范围为10×10~4~1.2×10~4pg·mL~(-1)(γ=0.9993),日内、日间RSD均小于10%,提取回收率约为80%。结论该方法快速、准确、灵敏度高,可用于氯吡格雷血药浓度测定。 相似文献