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1.
Sodium tanshinone IIA sulfonate (STS) is a water-soluble derivative of tanshinone IIa, an important lipophilic component contained in Salvia miltiorrhizae. A simple, sensitive and robust quantification method for STS based on LC-ESI-MS/MS was developed and validated, and has been successfully applied to the pharmacokinetic study. Liquid-liquid extraction was used for extracting STS from biological samples, with a satisfactory recovery exceeding 75% at all test concentrations. Isocratic mobile phase consisted of 75% acetonitrile and 25% water containing 0.005% ammonia acetate (pH 3). Good retention and baseline separation for STS and the selected internal standard, diclofenac sodium, were obtained on a Shim-pack VP-ODS analytical column under this condition. The method was linear in the concentration range of 1-500 ng/mL. The intra- and inter-day precisions (RSD%) were within 9.0%. The deviation of the assay accuracies was within +/-10.0%. STS was proved to be stable during all sample storing, preparation and analytic procedures. With a lower limit of quantitation at 1 ng/mL, this method has been proved to be sensitive enough for the pharmacokinetic study of STS. The plasma profile of STS followed a single intravenous dosing was well fitted to a three compartmental model. 相似文献
2.
Study of tanshinone IIA tissue distribution in rat by liquid chromatography-tandem mass spectrometry method 总被引:1,自引:0,他引:1
Bi HC Law FC Zhong GP Xu CS Pan Y Ding L Chen X Zhao LZ Xu Q Huang M 《Biomedical chromatography : BMC》2007,21(5):473-479
A liquid chromatography/tandem mass spectrometry (LC/MS/MS) method was developed and validated for determining tanshinone IIA in rat tissues. After a single step liquid-liquid extraction with diethyl ether, tanshinone IIA and loratadine (internal standard) was subjected to LC/MS/MS analysis using positive electro-spray ionization under selected reaction monitoring mode. Chromatographic separation of tanshinone IIA and loratadine was achieved on a Hypersil BDS C(18) column (i.d. 2.1 x 50 mm, 5 microm) with a mobile phase consisting of methanol-1% formic acid (90:10, v/v) at a flow rate of 300 microL/min. The intra-day and inter-day precision of the method were less than 10.2 and 12.4%, respectively. The intra-day and inter-day accuracies ranged from 99.7 to 109.7%. The lowest limit of quantification for tanshinone IIA was 1 ng/mL. The method was applied to a tanshinone IIA tissue distribution study after an oral dose of 60 mg/kg to rats. Tanshinone IIA tissue concentrations decreased in the order of stomach > small intestine > lung > liver > fat > muscle > kidneys > spleen > heart > plasma > brain > testes. Tanshinone IIA still could be detected in most of the tissues at 20 h post-dosing. These results indicate that the LC/MS/MS method was rapid and sensitive to quantify tanshinone IIA in different rat tissues. 相似文献
3.
Yiming Liu Aihua Lin Zhifeng Wu Runmei Ou Haiding Huang 《Biomedical chromatography : BMC》2010,24(2):174-179
A sensitive, rapid and specific liquid chromatography–electrospray ionization–tandem mass spectrometry method was developed and validated for the determination of aristolochic acid‐I (AA‐I) in rat plasma. Finasteride was used as the internal standard (IS). The analyte was separated on a Zorbax Eclipse XDB‐C18 column by isocratic elution with methanol‐10 mM ammonium acetate (75:25, v/v, pH = 7.3) at a flow rate of 0.25 mL/min, and analyzed by mass spectrometry in positive multiple reaction monitoring mode. The precursor‐to‐product ion transitions of m/z 359.0 → 298.2 and m/z 373.1 → 305.2 were used to detect AA‐I and IS, respectively. Good linearity was achieved over a range of 0.4–600 ng/mL. Intra‐ and inter‐day precisions measured as relative standard deviation were less than 13.5%, and accuracy ranged from 94.2 to 97.5%. The developed method was successfully applied in the pharmacokinetic study of AA‐I in rats. Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
4.
A sensitive, accurate, rapid and robust LC‐MS‐MS method for the quantification of aucubin, a major bioactive constituent of Aucuba japonica, Eucommia ulmoides and Plantago asiatica, was established and validated in rat plasma. Plasma samples were simply precipitated by adding methanol and the supernatant was chromatographed by a Diamonsil® C18(2) column with the mobile phase comprising a mixture of 10 mm ammonium acetate in methanol and that in water with the ratio of 50:50 (v/v). Quantification of aucubin was performed by mass spectrometry in the multiple‐reaction monitoring mode with positive atmospheric ionization at m/z 364 → 149 for aucubin, and m/z 380 → 165 for catalpol (IS), respectively. The retention time was 2.47 and 2.44 min for aucubin and the IS, respectively. The calibration curve (10.0–30,000 ng/mL) was linear (r2 > 0.99) and the lower limit of quantification was 10.0 ng/mL in the rat plasma sample. The method showed satisfactory results such as sensitivity, specificity, precision, accuracy, recovery, freeze–thaw and long‐term stability. This simple LC‐MS method was successfully applied in a pharmacokinetic study carried out in Sprague–Dawley rats after oral administration of aucubin at a single dose of 50 mg/kg. Herein the pharmacokinetic study of aucubin is reported for the first time. Copyright © 2011 John Wiley & Sons, Ltd. 相似文献
5.
The metabolism of tanshinone IIA was studied in rats after a single-dose intravenous administration. In the present study, 12 metabolites of tanshinone IIA were identified in rat bile, urine and feces with two LC gradients using LC-MS/MS. Seven phase I metabolites and five phase II metabolites of tanshinone IIA were characterized and their molecular structures proposed on the basis of the characteristics of their precursor ions, product ions and chromatographic retention time. The seven phase I metabolites were formed, through two main metabolic routes, which were hydroxylation and dehydrogenation metabolism. M1, M4, M5 and M6 were supposedly tanshinone IIB, hydroxytanshinone IIA, przewaquinone A and dehydrotanshinone IIA, respectively, by comparing their HPLC retention times and mass spectral patterns with those of the standard compounds. The five phase II metabolites identified in this research were all glucuronide conjugates, all of which showed a neutral loss of 176 Da. M9 and M12 were more abundant than other identified metabolites in the bile, which was the main excretion path of tanshinone IIA and the metabolites. M12 was the main metabolite of tanshinone IIA. M9 and M12 were proposed to be the glucuronide conjugates of two different semiquinones and these semiquinones were the hydrogenation products of dehydrotanshinone IIA and tanshinone IIA, respectively. This hydrogenized reaction may be catalyzed by the NAD(P)H: quinone acceptor oxidoreductase (NQO). The biotransformation pathways of tanshinone IIA were proposed on the basis of this research. 相似文献
6.
Kim SJ Koo TS Ha DJ Baek M Lee SK Shin DS Moon H 《Biomedical chromatography : BMC》2012,26(3):371-376
A rapid, simple and sensitive liquid chromatography–tandem mass spectrometry (LC/MS/MS) was developed for the determination of an antiepileptic drug, lacosamide, in rat plasma. The method involves the addition of acetonitrile and internal standard solution to plasma samples, followed by centrifugation. An aliquot of the supernatant was diluted with water and directly injected into the LC/MS/MS system. The separations were performed on column packed with octadecylsilica (5 µm, 2.0 × 50 mm) with 0.1% formic acid and acetonitrile as mobile phase, and the detection was performed on tandem mass spectrometry by the multiple‐reaction monitoring via an electrospray ionization source. The standard curve was linear over the concentration range from 0.3 to 1000 ng/mL. The lower limit of quantification was 0.3 ng/mL using 50 μL of rat plasma sample. The intra‐ and inter‐assay precision and accuracy were found to be less than 11.7 and 8.8%, respectively. The developed analytical method was successfully applied to the pharmacokinetic study of lacosamide in rats. Copyright © 2011 John Wiley & Sons, Ltd. 相似文献
7.
Shakya S Zhu H Ding L Du XL Qi XM Yang XL Yang ZL 《Biomedical chromatography : BMC》2012,26(1):109-114
A sensitive and rapid liquid chromatography–tandem mass spectrometry (LC‐MS/MS) method has been developed and validated for the determination of asperosaponin VI in beagle dog plasma using glycyrrhizic acid as the internal standard (IS). Plasma samples were simply pretreated with methanol for deproteinization. Chromatographic separation was performed on a Hedera ODS‐2 column using mobile phase of methanol–10 mm ammonium acetate buffer solution containing 0.05% acetic acid (71:29, v/v) at a flow rate of 0.38 mL/min. Asperosaponin VI and the IS were eluted at 2.8 and 1.9 min, respectively, ionized in negative ion mode, and then detected by multiple reaction monitoring. The detection used the transitions of the deprotonated molecules at m/z 927.5 → 603.4 for asperosaponin VI and m/z 821.4 → 645.4 for glycyrrhizic acid (IS). The assay was linear over the concentration range of 0.15–700 ng/mL and was successfully applied to a pilot pharmacokinetic study in beagle dogs. Copyright © 2011 John Wiley & Sons, Ltd. 相似文献
8.
Kyeong‐Ryoon Lee Sung Heum Choi Jin‐Sook Song Hyewon Seo Yoon‐Jee Chae Hwang Eui Cho Jin Hee Ahn Sung‐Hoon Ahn Myung Ae Bae 《Biomedical chromatography : BMC》2013,27(7):846-852
In this study, we developed a method for the determination of PF‐04620110 (2‐{(1r,4r)‐4‐[4‐(4‐amino‐5‐oxo‐7,8‐dihydropyrimido[5,4‐f][1,4]oxazepin‐6(5H)‐yl)phenyl]cyclohexyl}acetic acid), a novel diacylglycerol acyltransferase 1 (DGAT‐1) inhibitor, in rat plasma and validated it using liquid chromatography–tandem mass spectrometry (LC‐MS/MS). Rat plasma samples were processed following a protein precipitation method by using acetonitrile and were then injected into an LC‐MS/MS system for quantification. PF‐04620110 and imipramine (internal standard) were separated using a Hypersil Gold C18 column, with a mixture of acetonitrile and 10 mm ammonium formate (90:10, v/v) as the mobile phase. The ion transitions monitored in positive‐ion mode [M + H]+ of multiple‐reaction monitoring were m/z 397.0 → 260.2 for PF‐04620110 and m/z 280.8 → 86.0 for imipramine. The detector response was specific and linear for PF‐04620110 at concentrations within the range 0.05–50 µg/mL and the signal‐to‐noise ratios for the samples were ≥10. The intra‐ and inter‐day precision and accuracy of the method matched the acceptance criteria for assay validation. PF‐04620110 was stable under various processing and/or handling conditions. PF‐04620110 concentrations in the rat plasma samples could be measured up to 24 h after intravenous or oral administration of PF‐04620110, suggesting that the assay is useful for pharmacokinetic studies in rats. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
9.
Liquid chromatography mass spectrometry simultaneous determination of vindoline and catharanthine in rat plasma and its application to a pharmacokinetic study
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Chongliang Lin Jinzhang Cai Xuezhi Yang Lufeng Hu Guanyang Lin 《Biomedical chromatography : BMC》2015,29(1):97-102
Vinblastine and vincristine, both of which are bisindole alkaloids derived from vindoline and catharanthine, have been used for cancer chemotherapy; their monomeric precursor molecules are vindoline and catharanthine. A simple and selective liquid chromatography mass spectrometry method for simultaneous determination of vindoline and catharanthine in rat plasma was developed. Chromatographic separation was achieved on a C18 (2.1 × 50 mm, 3.5 µm) column with acetonitrile–0.1% formic acid in water as mobile phase with gradient elution. The flow rate was set at 0.4 mL/min. An electrospray ionization source was applied and operated in positive ion mode; selective ion monitoring mode was used for quantification. Mean recoveries were in the range of 87.3–92.6% for vindoline in rat plasma and 88.5–96.5% for catharanthine. Matrix effects for vindoline and catharanthine were measured to be between 95.3 and 104.7%. Coefficients of variation of intra‐day and inter‐day precision were both <15%. The accuracy of the method ranged from 93.8 to 108.1%. The method was successfully applied in a pharmacokinetic study of vindoline and catharanthine in rats. The bioavailability of vindoline and catharanthine were 5.4 and 4.7%, respectively. Copyright © 2014 John Wiley & Sons, Ltd. 相似文献
10.
Quantitative determination of enzalutamide,an anti‐prostate cancer drug,in rat plasma using liquid chromatography–tandem mass spectrometry,and its application to a pharmacokinetic study
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Ji‐Hye Song Tae‐Heon Kim Jong‐Woo Jung Nakjeong Kim Sung Hoon Ahn Sung‐Ook Hwang Nam Sook Kang Sung‐Eun Yoo Tae‐Sung Koo 《Biomedical chromatography : BMC》2014,28(8):1112-1117
This report details a method using liquid chromatography–tandem mass spectrometry (LC‐MS/MS) that allows one to determine the concentration of an atypical anticancer drug, enzalutamide, in rat plasma. Specifically, this method involves the addition of an acetonitrile and bicalutamide (internal standard) solution to plasma samples. Following centrifugation of this mixture, an aliquot of the supernatant was directly injected into the LC‐MS/MS system. Separation was achieved using a column packed with octadecylsilica (5 µm, 2.1 × 50 mm) with 10 mM ammonium acetate in acetonitrile as the mobile phase; detection was accomplished using MS/MS by multiple‐reaction monitoring via an electrospray ionization source. This method demonstrated a linear standard curve (r = 0.997) over a concentration range of 0.001–1 µg/mL, as well as an intra‐ and inter‐assay precision of 2.7 and 5.1%, respectively, and an accuracy range from 100.8 to 105.6%. The lower limit of quantification was 1.0 ng/mL in 50 μL of rat plasma sample. We also demonstrated that this analytical method could be successfully applied to the pharmacokinetic study of enzalutamide in rats. Copyright © 2014 John Wiley & Sons, Ltd. 相似文献
11.
An LC‐MS/MS method was developed for the simultaneous determination of vitexin and isovitexin in rat plasma, using puerarin as the internal standard (IS). Plasma samples extracted with protein precipitation procedure were separated on a Diamonsil® C18 column (150 × 4.6 mm, 5 µm) with a mobile phase composed of methanol and 0.1% formic acid (45:55, v/v). The detection was accomplished by multiple reaction monitoring mode in positive electrospray ionization source. The optimized mass transition ion‐pairs for quantitation were m/z 431.2 → 311.1 for vitexin and isovitexin, and m/z 415.1 → 295.1 for IS. The total run time was 7.5 min for each injection. The calibration curves were linear (r2 > 0.99) over the investigated concentration range (2.00–2000 ng/mL) and the lower limits of quantification were 2.00 ng/mL in rat plasma sample. The intra‐ and inter‐day relative standard deviations were no more than 14.9% and the relative errors were within the range of ?3.2–2.1%. The extraction recoveries for both compounds were between 89.3 and 97.3%. The robust LC‐MS/MS method was further applied in the pharmacokinetic study in Sprague–Dawley rats after oral administration of Santalum album L. leaves extract at a dose of 116 mg/kg. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
12.
A method has been developed for the simultaneous quantification of metformin (I) and glipizide (II) in human plasma. It is based on high-performance liquid chromatography with electrospray ionization tandem mass (LC-ESI-MS/MS) spectrometric detection in positive ionization mode. Phenformin (III) and gliclazide (IV) were used as internal standards for I and II, respectively. The MS/MS detection was performed in multiple reaction monitoring (MRM) mode. The precursor-product ion combinations of m/z 130 --> 71, 446 --> 321, 206 --> 60 and 324 --> 127 were used to quantify I, II, III and IV, respectively. This method was validated in the concentration ranges of 0.02-4 microg/mL for I and 0.004-0.8 microg/mL for II. It was utilized to support a clinical pharmacokinetic study after single dose oral administration of a combination of I and II. 相似文献
13.
Xu CL Chen JW Ju WZ Liu SJ Chen Y Chen ZP Xue P Chen HJ Li X 《Biomedical chromatography : BMC》2012,26(10):1210-1214
A rapid, sensitive and specific method using liquid chromatography with tandem mass spectrometric detection (LC‐MS) was developed for the analysis of sauchinone in rat plasma. Di‐O‐methyltetrahydrofuriguaiacin B was used as internal standard (IS). Analytes were extracted from rat plasma by liquid–liquid extraction using ethyl acetate. A 2.1 mm i.d. × 150 mm, 5 µm, Agilent Zorbax SB‐C18 column was used to perform the chromatographic analysis. The mobile phase was methanol–deionized water (80:20, v/v). The chromatographic run time was 7 min per injection and the flow‐rate was 0.2 mL/min. The tandem mass spectrometric detection mode was achieved with electrospray ionization interface in positive‐ion mode (ESI+). The m/z ratios [M + Na]+, m/z 379.4 for sauchinone and m/z 395.4 for IS were recorded simultaneously. Calibration curve were linear over the range of 0.01–5 µg/mL. The lowest limit of quantification was 0.01 µg/mL. The intra‐day and inter‐day precision and accuracy of the quality control samples were 2.94–9.42% and 95.79–108.05%, respectively. The matrix effect was 64.20–67.34% and the extraction recovery was 93.28–95.98%. This method was simple and sensitive enough to be used in pharmacokinetic research for determination of sauchinone in rat plasma. Copyright © 2011 John Wiley & Sons, Ltd. 相似文献
14.
Suresh P S Abhishek Dixit Sanjeev Giri Sriram Rajagopal Ramesh Mullangi 《Biomedical chromatography : BMC》2013,27(4):496-501
A highly sensitive and rapid bioanalytical method has been developed and validated for the estimation of indomethacin in rat plasma with liquid chromatography coupled to tandem mass spectrometry with electrospray ionization in the positive‐ion mode. The assay procedure involves a simple liquid–liquid extraction of indomethacin and phenacetin (internal standard, IS) from rat plasma with acetonitrile. Chromatographic separation was achieved with 0.2% formic acid–acetonitrile (25:75, v/v) at a flow rate of 0.60 mL/min on an Atlantis dC18 column with a total run time 3.0 min. The MS/MS ion transitions monitored were 357.7 → 139.1 for indomethacin and 180.20 → 110.10 for IS. Method validation and pharmacokinetic study plasma analysis were performed as per FDA guidelines and the results met the acceptance criteria. The lower limit of quantitation achieved was 0.51 ng/mL and the linearity was observed from 0.51 to 25.5 ng/mL. The intra‐ and inter‐day precisions were in the range of 1.00–10.2 and 5.88–9.80%, respectively. This novel method has been applied to an oral pharmacokinetic study in rats. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
15.
Simultaneous determination of propofol and remifentanil in rat plasma by liquid chromatography–tandem mass spectrometry: application to preclinical pharmacokinetic drug–drug interaction analysis
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Mohamed A. El Hamd Mitsuhiro Wada Rie Ikeda Shigeru Kawakami Naotaka Kuroda Kenichiro Nakashima 《Biomedical chromatography : BMC》2015,29(3):325-327
Propofol (Pro) is an ultra‐short‐acting hypnotic agent used for general anesthesia that has no analgesic properties. Remifentanil (Rem) is an ultra‐short‐acting opioid administered concomitantly as an analgesic with Pro. To evaluate the pharmacokinetic interactions between Pro and Rem, we developed and validated a method combining high‐performance liquid chromatography with tandem mass spectrometry for simultaneous determination of Pro and Rem. The proposed method was successfully used to study the pharmacokinetic interactions of Pro and Rem coadministered to rats. Copyright © 2014 John Wiley & Sons, Ltd. 相似文献
16.
Wang J Zhu X Peng Y Zha W Feng D Zhu Y Wan P Qi H He J Zhou J Sun J 《Biomedical chromatography : BMC》2012,26(11):1371-1376
A rapid and sensitive liquid chromatography/tandem mass spectrometry (LC‐MS/MS) method was developed and validated for the quantification of trans‐stilbene glycoside (SG) in rat plasma. As trans‐SG can be rapidly isomerized under light exposure, trans‐SG plasma samples were prepared in the dark and assayed immediately. Trans‐SG and internal standard were extracted by protein precipitation. Chromatographic separation was achieved on a C18 column with a gradient elution program. The detection of analytes was performed by negative ion via multiple reaction monitoring mode. The precursor‐to‐product ions of m/z 405.1 → 242.9 for trans‐SG and m/z 389.1 → 226.9 for polydatin (internal standard) were monitored. No interference of endogenous components was observed for any plasma samples that we studied.The method was linear over the concentration range of 1.0–1000.0 ng/mL with a good correlation coefficient. The lower limit of quantification was 1.0 ng/mL for trans‐SG. The intra and inter‐batch accuracy for trans‐SG in stable rat plasma samples ranged from 93.3 to 102.7% and the variation was less than 8.1%. The extraction recoveries of trans‐SG in rat plasma were from 102.8 to 112.4% and the matrix effects were also acceptable. This method was successfully applied to pharmacokinetic study of trans‐SG in rats after intravenous administration. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
17.
Xiaoli Wu Chuwen Li Qingguo Li Zhen Qin Yuyang Yi Jiannan Chen Xiaoping Lai Ziren Su 《Biomedical chromatography : BMC》2013,27(9):1092-1099
Pogostone is an important constituent of Pogostemon cablin (Blanco) Benth., and possesses various known bioactivities. A rapid, simple and sensitive liquid chromatography tandem mass spectrometry (LC‐MS/MS) method was developed for the analysis of pogostone in rat plasma using chrysophanol as internal standard (IS). The analytes were extracted with methanol and separated using a reversed‐phase YMC‐UltraHT Pro C18 column. Elution was achieved with a mobile phase consisting of methanol–water (75:25, v/v) for 5 min at a flow rate of 400 μL/min. The precursor/product transitions (m/z) under MS/MS detection with negative electrospray ionization (ESI) were 223.0 → 139.0 and 253.1 → 224.9 for pogostone and IS, respectively. The calibration curve was linear over the concentration range 0.05–160 µg/mL (r = 0.9996). The intra‐ and inter‐day accuracy and precision were within ±10%. The validated method was successfully applied to the preclinical pharmacokinetic investigation of pogostone in rats after intravenous (5, 10 and 20 mg/kg) and oral administration (5, 10 and 20 mg/kg). Finally, the oral absolute bioavailability of pogostone in rats was calculated to be 70.39, 78.18 and 83.99% for 5, 10 and 20 mg/kg, respectively. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
18.
Quantitative determination of euphol in rat plasma by LC‐MS/MS and its application to a pharmacokinetic study
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Xu Xie Yongning Li Dongna Gao Yu Zhang Yanbo Ren 《Biomedical chromatography : BMC》2014,28(9):1229-1234
Euphol is a potential pharmacologically active ingredient isolated from Euphorbia kansui. A simple, rapid, and sensitive method to determine euphol in rat plasma was developed based on liquid chromatography‐tandem mass spectrometry (LC‐MS/MS) for the first time. The analyte and internal standard (IS), oleanic acid, were extracted from plasma with methanol and chromatographied on a C18 short column eluted with a mobile phase of methanol–water–formic acid (95:5:0.1, v/v/v). Detection was performed by positive ion atmospheric pressure chemical ionization in selective reaction monitoring mode. This method monitored the transitions m/z 409.0 → 109.2 and m/z 439.4 → 203.2 for euphol and IS, respectively. The assay was linear over the concentration range 27–9000 ng/mL, with a limit of quantitation of 27 ng/mL. The accuracy was between –7.04 and 4.11%, and the precision was <10.83%. This LC‐MS/MS method was successfully applied to investigate the pharmacokinetic study of euphol in rats after intravenous (6 mg/kg) and oral (48 mg/kg) administration. Results showed that the absolute bioavailability of euphol was approximately 46.01%. Copyright © 2014 John Wiley & Sons, Ltd. 相似文献
19.
A sensitive and specific high‐performance liquid chromatography–electrospray ionization–tandem mass spectrometry (HPLC‐ESI‐MS/MS) method was developed and validated for determination of rupestonic acid in rat plasma. Protein precipitation method was used to extract rupestonic acid and the internal standard (IS) warfarin sodium from rats plasma. The chromatographic separation was performed on an Agela Venusil XBP Phenyl column with an isocratic mobile phase consisting of methanol–0.1% formic acid in water (40:60, v/v), pumped at 0.4 mL/min. Rupestonic acid and the internal standard (IS) warfarin sodium were detected at m/z 247.2 → 203.1 and 307.1 → 161.3 in positive ion and multiple reaction monitoring mode respectively. The standard curves were linear over the concentration range of 2.5–5000 ng/mL (r2 > 0.99). The within‐day and between‐day precision values for rupestonic acid at four concentrations were 4.7–5.7 and 4.4–8.7%, respectively. The method described herein was fully validated and successfully applied to the pharmacokinetic study after an intravenous administration of rupestonic acid in rats. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
20.
《Biomedical chromatography : BMC》2017,31(3)
A sensitive and reliable bioanalytical method was established for quantitati\ve and pharmacokinetic investigation of nine ginsenosides and seven bufadienolides in rat plasma after the oral administration of Shexiang Baoxin Pill by liquid chromatography–electrospray ionization tandem mass spectrometry, using tinidazole and digoxin as internal standards (ISTDs). All of the analytes and ISTDs obtained satisfactory recoveries by solid‐phase extraction using an Oasis HLB μElution Plate, which was eluted with methanol and ethyl acetate successively, and chromatographic separation was achieved on a Shim‐pack XR‐ODSIIcolumn (75 × 2.0 mm, 2.2 μm) with gradient elution using a mixture of acetonitrile–0.1% formic acid solution (v /v) as the mobile phase at a flow rate of 0.3 mL/min. Detection was carried out by a triple‐quadrupole tandem mass spectrometry with positive/negative ion switching multiple reaction monitoring mode. All analytes showed good linearity over a wide concentration range (r 2 > 0.99). The lower limit of quantification was in the range 0.625–12.5 ng/mL for bufadienolides and 2–5.5 ng/mL for ginsenosides, and the mean recoveries of all analytes were in the range 78.29–99.35%. The intra‐ and inter‐day precisions (RSD) were in the range 0.08–12.38% with the accuracies between 86.09 and 99.40%. The validated method was then successfully applied to pharmacokinetic study of the above 16 compounds in rat plasma. Pharmacokinetic results indicated that the developed extraction and analytical method could be employed as a rapid, effective technique for pharmacokinetic study of multiple components, especially various polarity that are difficult to extract simultaneously. 相似文献