[Determination of mitomycin C in rabbit plasma by ultra-high performance liquid chromatography-tandem mass spectrometry]
National Center for Safety Evaluation of Drugs, National Institutes for Food and Drug Control, Beijing 100176, China.Se pu = Chinese journal of chromatography / Zhongguo hua xue hui 02/2012; 30(2):154-9. DOI: 10.3724/SP.J.1123.2011.10034
An ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for the determination of mitomycin C (MMC) in rabbit plasma was established. The blank rabbit plasma sample solutions added with mitomycin C and triamcinolone acetonide (internal standard, IS) were prepared. The solutions containing MMC and IS were extracted from the plasma with ethyl acetate using liquid-liquid extraction method. A Hypersil Gold C18 column (50 mm x 2.1 mm, 1.9 microm) was employed and the column temperature was set at 35 degrees C. The isocratic elution of methanol and 0.1% (v/v) formic acid aqueous solution as mobile phase was performed at a flow rate of 0.2 mL/min, and a rapid separation was completed within 3 min. The electrospray was operated in the positive ionization mode and the MMC and IS were identified in selected reaction monitoring (SRM) mode. The monitoring ions of MMC and IS were m/z 335. 2 --> 242.2 and m/z 435.2 --> 397. 3/415.2, respectively, which were used to qualify and quantify the targets by the method of matrix-matched standard solution. The calibration curve showed good linearity within the mass concentrations of 1 to 1 000 microg/L (r = 0.997 8, weighting: 1/x2). The limit of detection (S/N = 3) was 0.2 microg/L. The recoveries were from 85% to 115% at the spiked levels of 1, 5, 100 and 800 microg/L, and the relative standard deviations (RSDs) of intra- and inter-day were both less than 15%. The method can meet the determination requirements of biological samples, and can be used for the determination of mitomycin C in rabbit plasma after the administration of mitomycin C. The method is selective, sensitive, convenient, rapid and reproducible in the determination of mitomycin C, and also can be used for the pharmacokinetics research of mitomycin C in plasma.
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ABSTRACT: Aim: To administer mitomycin C-polylactide gel by being held on the ectotheca of rabbit and establish an ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for the determination of sustained-release quantity of mitomycin C in rabbit. Methods: 30 rabbits were given 0.05, 0.1, 0.2, 0.4 and 0.6 mg mitomycin C in 0.2 ml polylactide gel after the administration of a single ectotheca dose. The rabbit plasma samples added with mitomycin C and the internal standard (triamcinolone acetonide) standard solution was prepared. Ethyl acetate was added in the samples for the pretreatment and drug plasma concentration was determined by UHPLC-MS/MS. Results: The calibration curve showed good linearity within the concentrations of 1 to 1 000 μg·L -1 (r=0.9977, Weighing; 1/x 2); the limit of detection (S/N = 3 ) was 0.2 μg·L -1. The mean recoveries were from 85% to 115% at the spiked levels of 1, 5, 100 and 800 μg·L -1; the relative standard deviations (RSDs) of intra- and inter-day of variation were both less than 15%, which could meet the determination requirements of biological samples. After a single dose administration of ectotheca, sustained-release quantity of mitomycin C was little, drug plasma concentration was very low, which was a significant basis for applying UHPLC-MS/MS. Conclusions: The method is convenient, rapid, sensitive, selective and reproducible in the determination of mitomycin C, and can be used for the quantitative analysis of large biosamples and the pharmacokinetical study of mitomycin C. It is not easy to absorb MMC-PLA in body, and MMC-PLA has no effect on the whole body.Chinese Pharmacological Bulletin 05/2012; 28(5):721-725. DOI:10.3969/j.issn.1001-1978.2012.05.028
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ABSTRACT: An ultra-performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS) method was developed for the determination of alpha-solanine, alpha-chaconine and solanidine in plasma and urine. The sample was acidified with aqueous solution containing 2% (v/v if not specified) formic acid, and then cleaned-up by solid-phase extraction with a mixed-mode cation exchange (MCX) cartridge. The analysis of the glycoalkaloids was carried out on an Acquity UPLC BEH C18 column (50 mm x 2.1 mm, 1.7 microm) with gradient elution of acetonitrile (containing 0.1% formic acid) and H2O (containing 0.05% formic acid and 5.0 mmol/L ammonium acetate). The analytes were detected by positive electrospray ionization tandem mass spectrometry in MRM mode, and quantified by external matrix-matched standard calibration. The cycle time of each analysis was 5.5 min. The calibration curves were linear in the range of 0.3-100 ng/mL of the glycoalkaloids in plasma and urine. The correlation coefficients were 0.997-0.999. The limits of detection (S/N = 3) and quantitation (S/N = 10) were 0.1 ng/mL and 0.3 ng/mL. The average recoveries were 82%-112% and 96%-114% for the glycoalkaloids spiked in plasma and urine, respectively, with relative standard deviations of 4.0%-16% and 2.7%-17% (n = 6). The method is simple, accurate and sensitive to detect the glycoalkaloids in plasma and urine for both clinical and forensic purposes.Se pu = Chinese journal of chromatography / Zhongguo hua xue hui 06/2014; 32(6):586-90. DOI:10.3724/SP.J.1123.2014.03001
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ABSTRACT: In the history of medicine, nature has represented the main source of medical products. Indeed, the therapeutic use of plants certainly goes back to the Sumerian and Hippocrates and nowadays nature still represents the major source for new drugs discovery. Moreover, in the cancer treatment, drugs are either natural compounds or have been developed from naturally occurring parent compounds firstly isolated from plants and microbes from terrestrial and marine environment. A critical element of an anticancer drug is represented by its severe toxicities and, after administration, the drug concentrations have to remain in an appropriate range to be effective. Anyway, the drug dosage defined during the clinical studies could be inappropriate for an individual patient due to differences in drug absorption, metabolism and excretion. For this reason, personalized medicine, based on therapeutic drug monitoring (TDM), represents one of most important challenges in cancer therapy. Mass spectrometry sensitivity, specificity and fastness lead to elect this technique as the Golden Standard for pharmacokinetics and drug metabolism studies therefore for TDM. This review focuses on the mass spectrometry-based methods developed for pharmacokinetic quantification in human plasma of anticancer drugs derived from natural sources and already used in clinical practice. Particular emphasis was placed both on the pre-analytical and analytical steps, such as: sample preparation procedures, sample size required by the analysis and the limit of quantification of drugs and metabolites to give some insights on the clinical practice applicability. © 2015 Wiley Periodicals, Inc. Mass Spec Rev. © 2015 Wiley Periodicals, Inc.Mass Spectrometry Reviews 08/2015; DOI:10.1002/mas.21478 · 7.71 Impact Factor
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