共查询到20条相似文献，搜索用时 15 毫秒
1.
Sebastian P. A. Rosser Caroline Atkinson Christa E. Nath Jamie I. Fletcher 《Journal of separation science》2022,45(14):2508-2519
A liquid chromatography-tandem mass spectrometry method was developed and validated for the simultaneous quantification of vincristine and tariquidar in 10 μL of mouse whole blood using volumetric absorptive microsampling devices. Samples were extracted from the devices and quantified against calibrators prepared in a human blood plasma matrix. Separation of vincristine and tariquidar was achieved using a Shimpack XR ODS III C18 stationary phase and H2O and methanol mobile phase solvents containing 0.1% formic acid, running a gradient elution at a flow rate of 0.2 mL/min over 6.0 min. The method was linear up to 1200 ng/mL (R2 > 0.99 for both analytes), with calibrator accuracy within ± 15% of the nominal concentrations and analyte coefficient of variance <15% for both vincristine and tariquidar. Pharmacokinetic assessment of both analytes was successfully applied in mice as both single-agent therapy and combination therapy over a 24-h period, and a 2.3-fold increase in vincristine drug exposure was observed in combination with tariquidar. This study validates the use of this approach for longitudinal analysis of drug exposure in animal studies. 相似文献
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3.
Kai-Chun Chang 《液相色谱法及相关技术杂志》2018,41(8):445-450
The bioequivalence of two Florfenicol (FF) products in pigs was evaluated. A 2?×?2 crossover trial with a 14 days wash-out period was performed. The pigs were orally administered in a single dose (2?mg/kg b.w of FF). Serum samples were analyzed using a liquid chromatography-tandem mass spectrometry method. The limit of quantification was 0.1?ng/mL, and the calibration range was 1.0–100.0?ng/mL. Furthermore, intraday and interday were 5.43–9.09% and 6.23–9.68%, respectively. The areas under the curve (AUC0–48) for the test product B of FF and reference product A were 7289.61?±?1750.44 and 6545.01?±?2766.25?h?×?ng/mL, respectively. The highest concentrations of FF in the serum (Cmax) were 726.05?±?211.77 and 641.97?±?117.94?ng/mL. The mean retention times (MRT) was 7.91?±?1.98 and 7.76?±?2.89?h while the half-lives (T1/2) were 4.07?±?1.71 and 4.99?±?3.30?h. From the analysis of variance results, the p values of Cmax and AUC0–∞ for the 90% confidence interval were 0.492 and 0.320 (p?>?0.05), respectively. A comparison between the test product and the reference product showed no significant difference. Both products showed bioequivalence after being administered in pigs. 相似文献
4.
瑞芬太尼在人体中的代谢动力学研究 总被引：3，自引：0，他引：3
建立了用液相色谱-串联质谱技术进行瑞芬太尼代谢动力学研究的方法。比较了不同停药时间对瑞芬太尼浓度及代谢产物的影响。瑞芬太尼浓度测定采用串联质谱的选择反应监测技术,以m/z377>345为定量离子对,定量检出限为0.5μg/L。代谢产物的测定采用液质联用技术,同时测定二级质谱。在停药8min后,瑞芬太尼代谢90%。氧化和水解是瑞芬太尼的主要代谢反应,瑞芬太尼在人体中形成4种代谢物。该研究方法简单、快速、灵敏,具有广泛的应用性。 相似文献
5.
Xinyue Zheng Xujian Duan Di Lu Qiuhong Jiang Yajun Liu Hongyu Xue Jiansong You Lei Yin Meiyun Shi 《Journal of separation science》2023,46(1):2200725
Butachlor is an aromatic amide compound that plays a role as a herbicide, a xenobiotic, and an environmental contaminant. The aim of this work was to develop a highly selective and sensitive ultra-performance liquid chromatography-tandem mass spectrometry method based on the tandem mass spectrometry cubed technique to determine butachlor in a biological matrix. Butachlor and internal standard acetochlor were separated on a Waters Acquity ultra-performance liquid chromatography BEH C18 column (2.1 × 50 mm, 1.7 μm) with gradient elution using 0.1% formic acid aqueous solution (A) and acetonitrile (B) as mobile phases. The transitions selected for tandem mass spectrometry cubed quantitative analysis in positive ion mode were: for butachlor, mass-to-charge ratio 312.2→238.1→162.1; for acetochlor, mass-to-charge ratio 270.1→224.0→148.1. The total running time for each sample was 5.5 min. The ultra-performance liquid chromatography-tandem mass spectrometry cubed method showed a linear relationship (R2 ≥ 0.995) in the concentration range of 0.5–100 ng/ml. The intra and interday accuracies are within the range of -10.6%–4.3% and precisions are between 4.48% and 13.14%. The novelty of the method is the use of tandem mass spectrometry cubed scanning mode, which improves selectivity and sensitivity. The results indicated that butachlor was cellular toxic. The safety of butachlor should be considered when it is used as a herbicide. 相似文献
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Zhi Zhang Runzhi Li Shihao Liu Lei Yin Tongtong Xu John Paul Fawcett Jingkai Gu 《Journal of separation science》2019,42(18):3033-3040
Alarelin, a gonadotropin‐releasing hormone analogue, is widely used in China for the treatment of endometriosis and uterine leiomyoma. In order to investigate its pharmacokinetic behavior and support the preclinical application of new formulations, we have developed a novel and highly selective bioanalytical method to determine alarelin in rat plasma based on liquid chromatography tandem mass spectrometry with triple stage fragmentation. After sample preparation by protein precipitation followed by reversed phase solid phase extraction, alarelin and triptorelin (internal standard) were chromatographed on an Ascentis® Express C18 column (50 mm × 4.6 mm, 2.7 µm) using gradient elution with 0.1% formic acid in water and acetonitrile at a flow rate of 1 mL/min. Detection was by positive mode electrospray ionization followed by triple stage fragmentation using the transitions at m/z 584.6→249.1→221.0 for alarelin and 656.5→249.1→176.0 for triptorelin, The assay was linear in the concentration range 0.3‐10 ng/mL with excellent precision and accuracy. It was successfully applied to a pharmacokinetic study in rats administered a dose of 13.5 µg/kg alarelin by intramuscular injection. The results show that the triple stage fragmentation strategy allows highly selective analysis of alarelin and has the potential to be widely applied to the bioassay of other peptidic drugs. 相似文献
7.
Praveen Kumar Kondaveti;Paul Douglas Sanasi;G Saravanan;Koti Reddy Yeruva;Mahesh Palla; 《SEPARATION SCIENCE PLUS》2024,7(12):e202400186
The objective of the study is to develop a sensitive and simple liquid chromatography-tandem mass spectrometry for the determination of nine azido impurities in Losartan potassium active pharmaceutical ingredients. An advanced analytical method should be developed to determine these nine Azido impurities at 0.5 ppm level. Currently, no such method is reported to control these impurities in losartan potassium drug substance. The nine impurities separation was achieved using Hypersil ODS stationary phase with gradient elution and mobile phase of 0.1 M ammonium acetate as mobile phase A and methanol as mobile phase B. The developed method was found to be sensitive to the limit of detection and limit of quantitation levels as per the International Council for Harmonization M7 guidelines. The method was linear from 0.5 ppm to 15 ppm for all nine azido impurities. This is a single method for the simultaneous determination of all azido impurities in the presence of losartan potassium drug substance at 0.5 ppm and the same method used in the quality control laboratory for sample analysis. 相似文献
8.
Walczak M Kozaczek E Szymura-Oleksiak J Pękala E 《Biomedical chromatography : BMC》2011,25(3):381-390
A sensitive and selective liquid chromatographic–electrospray ionization mass spectrometric method for the simultaneous determination of propentofylline and enantiomers of its active metabolite M1 in rat serum, cortex and hippocampus was developed and validated according to GLP procedures. Sample preparations were carried out by liquid–liquid extraction using diethyl ether after the addition of the internal standard (pentoxifylline). The dried residue was reconstituted in mobile phase and injected onto a Chiralpak AD column (10 µm, 250 × 4.6 mm i.d.). The limit of quantification for propentofylline in serum, cortex and hippocampus was set at 0.25 ng/mL and for enantiomers of its metabolite M1 at 1.25 ng/mL. The established LC/ESI‐MS/MS method has been successfully applied to an initial pharmacokinetic study of propentofylline and also to assessment of distribution of parent drug and enantiomers of its pharmacologically active metabolite M1 to cortex and hippocampus after intravenous administration of propentofylline to rats at a dose of 5 mg/kg. Copyright © 2010 John Wiley & Sons, Ltd. 相似文献
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液相色谱-串联质谱法与气相色谱-串联质谱法测定茶叶中苦参碱残留量 总被引：2，自引：0，他引：2
建立了茶叶中苦参碱残留检测的两种前处理方法,比较了液相色谱-串联质谱(LC-MS/MS)与气相色谱-串联质谱(GC-MS/MS)检测茶叶中苦参碱残留量分析方法的适用性。结果表明,在添加标准样品10100μg/kg3个水平时,两种前处理方法的回收率和精密度无显著差别;GC-MS/MS和LC-MS/MS回收率分别为81%85%、82%86%,相对标准偏差(RSD)分别为4.6%11.5%和2.9%4.2%。结果表明两种样品前处理方法以及LC-MS/MS与GC-MS/MS检测均能满足茶叶中苦参碱残留量的测定,但采用前处理方法二,LC-MS/MS检测茶叶中苦参碱残留更具优势。 相似文献
10.
Seshulatha Jamalapuram Pradeep Kumar Vuppala Ahmed H. Abdelazeem Christopher R. McCurdy Bonnie A. Avery 《Biomedical chromatography : BMC》2013,27(8):1034-1040
Methamphetamine abuse continues as a major problem in the USA owing to its powerful psychological addictive properties. AZ66, 3‐[4‐(4‐cyclohexylpiperazine‐1‐yl)pentyl]‐6‐fluorobenzo[d]thiazole‐2(3H)‐one, an optimized sigma receptor ligand, is a promising therapeutic agent against methamphetamine. To study the in vivo pharmacokinetics of this novel sigma receptor ligand in rats, a sensitive ultra‐performance liquid chromatography/tandem mass spectrometry (UPLC/MS/MS) method was developed in rat plasma and validated. The developed method requires a small volume of plasma (100 μL) and a simple liquid–liquid extraction. The chromatographic separations were achieved in 3.3 min using an Acquity UPLC BEH Shield RP18 column. The mass spectrophotometric detection was carried out using a Waters Micromass Quattro MicroTM triple‐quadrupole system. Multiple reaction monitoring was used for the quantitation with transitions m/z 406 → m/z 181 for AZ66 and m/z 448 → m/z 285 for aripiprazole. The method was validated over a concentration range of 1–3500 ng/mL and the lower limit of quantitation was determined to be 1 ng/mL. Validation of the assay demonstrated that the developed UPLC/MS/MS method was sensitive, accurate and selective for the determination of AZ66 in rat plasma. The present method has been successfully applied to an i.v. pharmacokinetic study in Sprague–Dawley rats. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
11.
《液相色谱法及相关技术杂志》2012,35(2):116-128
A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the determination of fosfomycin in chicken serum using fudosteine as the internal standard. Serum samples were treated with methanol to precipitate proteins. A subsequent clean up using liquid-liquid extraction followed by dilution was performed to eliminate phospholipids which are prone to produce unwanted matrix effects. The HPLC-MS/MS system involved the use of an isocratic mobile phase on a cyano stationary phase column and electrospray ion source operating in negative ion mode. Single reaction monitoring of transitions m/z 137 →79 and 178 →91 was performed on a triple quadrupole mass spectrometer to quantify fosfomycin and fudosteine, respectively. Response was linear over the range of 0.1 to 50 μg mL−1. Recovery ranged from 95 to 108%. Accuracy determined for spiked samples at 5, 10, and 20 μg mL−1 was −7.8, 1 and −0.7%, respectively, expressed as relative error. Within day and between days precision, in terms of coefficient of variation, were less than 10% for all concentrations. The developed method was successfully used in a pharmacokinetic study after oral administration of calcium fosfomycin to broiler chickens. 相似文献
12.
建立了测定人血浆中卡托普利的LC/MS/MS法。取血浆0.2 mL,用对溴苯甲酰甲基溴进行衍生化,经甲醇沉淀蛋白后,以甲醇-10 mmol/L乙酸铵-甲酸(80/20/0.4,V/V)为流动相,用Zorbax SB-C18柱分离,通过配有电喷雾离子化源的四极杆-线性离子阱质谱仪,以多反应监测(MRM)方式进行检测。用于定量分析的离子反应分别为m/z416→m/z216(卡托普利衍生物)和m/z28→m/z193(安定)。卡托普利的线性范围为2.5~1000μg/L,最低定量限为2.5μg/L,样品分析时间为2.0 m in。该法精密、准确,在灵敏度和分析速度上优于以往文献报道,适用于游离型卡托普利血药浓度的监测和药动学研究。 相似文献
13.
高效液相色谱-串联质谱联用测定脂肪中乙酰孕激素残留 总被引：6，自引：0，他引：6
建立了脂肪中5种乙酰孕激素,包括醋酸甲羟孕酮(MPA)、醋酸氯地孕酮(CMA)、醋酸甲地孕酮(MEGA)、甲烯雌醇醋酸酯(MLA)及17α-羟基孕酮醋酸酯(HPA)的液相色谱-串联质谱(LC-MS/MS)检测方法。考察了脂肪样品溶剂提取、固相萃取净化对样品分析的影响,确定样品各前处理过程的条件。采用电喷雾(ESI)阳离子,在选择反应监测模式(SRM)下,本方法对5种乙酰孕激素的检出限为0.2～0.3μg/kg,定量限为0.5μg/kg。在空白猪脂肪样品中以0.5、1.0和5.0μg/kg3个水平添加时,5种乙酰孕激素的回收率范围在60.5%～84.1%,RSD为8.9%～16.8%。 相似文献
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运用高效液相色谱-串联质谱联用技术,建立了简单、快速、灵敏的比格犬灌胃莫诺苷后血药浓度的检测方法。血浆样品采用蛋白质沉淀法处理,以芍药苷作为内标,色谱柱为Inertsil ODS-SP色谱柱(50 mm×2.1 mm,5μm),流动相为水(含1 mmol/L甲酸钠)-乙腈,梯度洗脱,流速0.4 mL/min。采用电喷雾离子源(ESI),正离子多反应监测(MRM)模式。绘制血药浓度-时间曲线,并采用DAS 2.0软件计算药代动力学参数。方法学实验结果表明内源性杂质不干扰莫诺苷和内标的测定,线性范围为2~5 000μg/L(r=0.996 6),定量限为2μg/L。方法精密度、准确度、回收率和基质效应均符合生物样品测定的要求,适合比格犬血浆中莫诺苷浓度的测定,可以应用该方法进行莫诺苷的药代动力学研究。比格犬灌胃莫诺苷3个剂量(5、15、45 mg/kg)后的血药浓度-时间曲线下面积(AUC(0-∞))分别为(1 631.20±238.50)、(3 984.05±750.38)、(10 397.64±3 156.34)μg/L·h,与给药剂量之间呈现良好的线性关系。 相似文献
15.
液相色谱串联质谱法定量检测青花菜中L-硒甲基硒代半胱氨酸 总被引：9，自引：0，他引：9
建立了液相色谱串联质谱(LC-MS-MS)法测定青花菜中L-硒甲基硒代半胱氨酸(SeMC)含量的方法。植物样品经沸水提取,以甲醇-0.1%七氟丁酸水溶液(30∶70)为流动相,滤液经Waters Symmetry C18(50 mm×3.9 mm,5μm)分离,经在线电喷雾离子源(ESI)正离子化后,采用多反应离子监测方式(MRM)选择m/z184.0→(167.0,94.9)测定SeMC。SeMC的线性范围为0-200 mg/L,准确度在96%-114%之间,日内日间精密度(RSD)在±10%内。检出限为0.1 mg/kg。结果表明:本方法高效、准确,特异性强,样品处理简单,可准确定量富硒青花菜中的SeMC。 相似文献
16.
液相色谱–串联质谱法测定草莓中二噻农残留 总被引：1，自引：0，他引：1
采用盐酸酸化乙腈提取草莓中二噻农残留,提取溶液经无水硫酸钠和PSA净化后,利用安捷伦Poroshell120 EC–C18色谱柱进行分离,以甲醇–水(体积比20∶80,含5 mmol/L乙酸铵溶液)作为流动相,ESI负离子模式下进行液相色谱–四极杆串联质谱分析。结果表明,在10~200μg/L浓度范围内,线性关系良好,r20.999 8,平均回收率为71.8%~78.3%,相对标准偏差小于5%(n=6),方法定量限为5μg/kg。该方法简单快速,可满足新鲜草莓中二噻农残留检测工作的需要。 相似文献
17.
建立苹果中水胺硫磷残留的液相色谱-串联质谱检测方法。样品以乙腈提取,采用电喷雾正离子源(ESI~+)和多重反应监测(MRM)模式测定,基质匹配标准曲线定量。结果表明:苹果基质中,水胺硫磷色谱峰面积响应值与其质量浓度呈良好线性关系(r~2=0.999),方法的线性范围为0.3~100μg/L,检出限为0.15μg/L,定量限为0.5μg/L。在5,50,100μg/kg添加水平下,水胺硫磷回收率为77.3%~95.2%,测定结果的相对标准偏差为5.7%~8.9%(n=6)。方法精密度和准确度满足残留限量监测要求。 相似文献
18.
液相色谱-串联质谱法鉴定大鼠血浆中的东莨菪碱及其代谢物 总被引：1，自引：0，他引：1
建立了鉴别东莨菪碱及其代谢物的液相色谱-电喷雾离子阱串联质谱(LC-MSn)联用方法。取单剂量灌胃50 mg/kg东莨菪碱的大鼠血样,甲醇沉淀蛋白,采用LC-MS及LC-MSn等方法分析血样。和空白血样及东莨菪碱相比较,根据血样中代谢物分子量的变化(ΔM)及其多级质谱数据,鉴定并阐述其结构。结果在服药后的大鼠血样中发现7种代谢物,分别为莨菪品、N-去甲基莨菪品、脱水东莨菪碱,N-去甲基脱水东莨菪碱、N-去甲基东莨菪碱、氧化东莨菪碱以及托品酸等。该方法灵敏,快速,简便,适合于药物及其代谢物的快速鉴定。 相似文献
19.
电喷雾串联质谱法分析阿托品及其代谢物 总被引：2，自引：0，他引：2
应用液相色谱-电喷雾串联质谱(LC-MSn)法检测阿托品及其大鼠粪样中的代谢物。收集灌胃25mg/kg阿托品的大鼠粪样,以水浸泡后,用乙酸乙酯萃取,采用LC-MS及LC-MSn等方法检测原药及其代谢物。和空白粪样及阿托品相比较,依据保留时间、一级质谱和二级质谱数据,在服药后的大鼠粪样中发现9种代谢物,分别为托品、N-去甲基托品、N-去甲基脱水阿托品、脱水阿托品、N-去甲基阿托品、羟基阿托品、N-氧化阿托品、羟基甲氧基阿托品以及托品酸等。该方法快速,简便,适合于生物样品中药物代谢物的快速鉴定。 相似文献
20.
Dun-Jian Wang Da-Wei Wang Qiu-Chen Fang Ye Shen Nv-Jin Zeng Yan-Ling Yang Hong-Wen Zhang Yong-Qing Wang Lu-Ning Sun 《Journal of separation science》2022,45(6):1146-1152
Regadenoson, the first selective adenosine A2A receptor agonist, is used to perform exercise stress test during radionuclide myocardial perfusion imaging. To detect the concentration of regadenoson in human plasma, a simple, fast, and sensitive tandem mass spectrometry method was established herein. Acetonitrile was used as a protein precipitation agent. Chromatographic separation was completed in 6.5 min using a BEH HILIC column (50 × 2.1 mm, 1.7 μm). The mobile phase consisted of 10 mmol/L ammonium acetate/acetonitrile (gradient elution). To quantify regadenoson and regadenoson-d3, an API 4000 mass spectrometry in multiple reaction monitoring mode with transitions of 391.3→259.2 and 394.3→262.2, respectively, was utilized. The calibration curve was linear in the range of 0.100–50.0 μg/L, and the intrabatch and interbatch precisions were <9.7% and <13.0%, respectively, and the accuracy was 2.0–6.9%. There was no apparent matrix effect for regadenoson or regadenoson-d3. The developed method was used to study the pharmacokinetic characteristics of regadenoson in healthy Chinese subjects. 相似文献