scholarly journals Pharmacokinetics study of potential anti-CML drug Cyclobentinib (CB1107) by HPLC–MS/MS

2021 ◽  
Vol 3 (1) ◽  
pp. 169-175
Author(s):  
Xinghua Zhao ◽  
◽  
Jiaojiao Zhang ◽  
Yutong Liang ◽  
Jie Li ◽  
...  
Keyword(s):  
Formic Acid ◽  
Mobile Phase ◽  
Time Curve ◽  
Column Temperature ◽  
Mobile Phases ◽  
Ionization Reaction ◽  
Liquid Chromatography Tandem Mass ◽  
Different Doses

Purpose: A simple, sensitive and specific HPLC–MS/MS method was established to analysis the pharmacokinetics of CB1107 in mouses. Methods: A simple, selective, and sensitive high-throughput liquid chromatography-tandem mass spectrometry (LC-MS-MS) method has been developed and validated for quantitative determination of CB1107 in rat serum.Chromatographic separation was achieved on a Zorbax Extend C18 Rapid Resolution HD column (4.6 mm × 50 mm, 1.8 μm). The column temperature was maintained at 35℃ and at flow rate of 0.6 mL/min. Injection volume was 20 μL. The mobile phases consisted of 0.1% formic acid in water (mobile phase A)and 0.1% formic acid in acetonitrile (mobile phase B), and total run time was 30min. MS-MS detection was performed in the selected monitoring mode of electrospray positive ionization reaction. Results: The pharmacokinetic characteristics of CB1107 in mice belong to the two-compartment model.When the doses were 400 mg/kg, 600 mg/kg and 800 mg/kg, corresponding area under the plasma concentration-time curve (AUC) respectively were 20.011±1.24 mg/h/L, 26.778±2.19 mg/h/L, 38.82±1.44 mg/h/L, suggesting that CB1107 have a good absorption in the body.And the AUC of three doses are proportional, indicating that CB1107 conforms to linear pharmacokinetics in vivo. Conclusion: This method was successfully applied to study the pharmacokinetics at three different doses of CB1107 after oral administration in mouses. In this study, the bioactivity mechanism of CB1107, by the pharmacokinetic investigation of CB1107 in vivo.

scholarly journals Development and validation of an LC-MS/MS method for the determination of adapalene in pharmaceutical forms for skin application

2016 ◽  
Vol 81 (10) ◽  
pp. 1171-1181 ◽  
Author(s):  
Vladimir Dobricic ◽  
Natasa Bubic-Pajic ◽  
Bojan Markovic ◽  
Sote Vladimirov ◽  
Snezana Savic ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Ammonium Acetate ◽  
Intermediate Precision ◽  
Column Temperature ◽  
Mobile Phases ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Chromatographic Parameters ◽  
Development And Validation

Development and validation of a liquid chromatography - tandem mass spectrometry (LC-MS/MS) method for the determination of adapalene in pharmaceutical forms for skin application were presented. The MS/MS analysis of adapalene was performed by use of three mobile phases, consisted of acetonitrile and (a) 0.1 % formic acid, (b) 0.1 % trifluoroacetic acid and (c) 20 mM ammonium acetate. The strongest signals of parent ion and dominant product ion were obtained in negative mode by use of the mobile phase (c). Validation of this method was performed according to the ICH guidelines. Small variations of selected chromatographic parameters (concentration of ammonium acetate, mobile phase composition, column temperature and flow rate) did not affect qualitative and quantitative system responses significantly, which proved method?s robustness. The method is specific for the determination of adapalene. Linearity was proved in the concentration range 6.7 - 700.0 ng mL-1 (r = 0.9990), with limits of detection and quantification 2.0 ng mL-1 and 6.7 ng mL-1, respectively. Accuracy was confirmed by calculated recoveries (98.4 % - 101.5 %). Precision was tested at three levels: injection repeatability, analysis repeatability and intermediate precision. Calculated relative standard deviations were less than 1, 2 and 3 %, respectively.

scholarly journals Determination of Levamisole and Mebendazole and Its Two Metabolite Residues in Three Poultry Species by HPLC-MS/MS

Foods ◽  
2021 ◽  
Vol 10 (11) ◽  
pp. 2841
Author(s):  
Pengfei Gao ◽  
Peiyang Zhang ◽  
Yawen Guo ◽  
Zhaoyuan He ◽  
Yuhao Dong ◽  
...  
Keyword(s):  
High Performance ◽  
Solid Phase ◽  
Gradient Elution ◽  
Column Temperature ◽  
Mobile Phases ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass ◽  
Peak Areas

A high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed to simultaneously analyze levamisole (LMS) and mebendazole (MBZ) and its two metabolites, 5-hydroxymebendazole (HMBZ) and 2-amino-5-benzoylbenzimidazole (AMBZ), in poultry muscle (chicken, duck and goose). In the sample preparation process, basic ethyl acetate was used as the extraction agent, and the extracted samples were back-extracted with hydrochloric acid, purified by Oasis MCX solid-phase extraction (SPE) cartridges, and reconstituted in the initial mobile phase after being blown dry with nitrogen. Chromatographic separation was performed on an Xbridge C18 column (4.6 mm × 150 mm, 5 μm) with 0.1% formic acid in water and acetonitrile as the mobile phases, and gradient elution was performed at a flow rate of 0.6 mL/min and a column temperature of 35 °C. In blank poultry muscle samples, the spiked concentrations of LMS, MBZ, HMBZ, and AMBZ were within the range of the limit of quantitation (LOQ) to 25 μg/kg. The peak areas of the four target drugs had a good linear relationship with the concentration, and the determination coefficient (R2) values were higher than 0.9990. The average recoveries of LMS, MBZ, HMBZ, and AMBZ were 86.77–96.94%; the intraday relative standard deviations (RSDs) were 1.75–4.99% at LOQ, 0.5 maximum residue limit (MRL), 1.0 MRL, and 2.0 MRL; the interday RSDs were 2.54–5.52%; and the LODs and LOQs were 0.04–0.30 μg/kg and 0.12–0.80 μg/kg, respectively.

Development and Pharmacokinetics Study of Antifungal Peptide Nanoliposomes by Liquid Chromatography-tandem Mass Spectrometry

2019 ◽  
Vol 15 (4) ◽  
pp. 312-318
Author(s):  
Shuoye Yang
Keyword(s):  
Mass Spectrometry ◽  
Biological Properties ◽  
Pharmacokinetic Property ◽  
Antifungal Peptide ◽  
Simple Liquid ◽  
Physico Chemical ◽  
Liquid Chromatography Tandem Mass ◽  
Pegylated Lipids

Background: The therapeutic ability and application of antifungal peptide (APs) are limited by their physico-chemical and biological properties, the nano-liposomal encapsulation would improve the in vivo circulation and stability. </P><P> Objective: To develop a long-circulating liposomal delivery systems encapsulated APs-CGA-N12 with PEGylated lipids and cholesterol, and investigated through in vivo pharmacokinetics. Methods: The liposomes were prepared and characterized, a rapid and simple liquid chromatographytandem mass spectrometry (LC-MS/MS) assay was developed for the determination of antifungal peptide in vivo, the pharmacokinetic characteristics of APs liposomes were evaluated in rats. Results: Liposomes had a large, unilamellar structure, particle size and Zeta potential ranged from 160 to 185 nm and -0.55 to 1.1 mV, respectively. The results indicated that the plasma concentration of peptides in reference solutions rapidly declined after intravenous administration, whereas the liposomeencapsulated ones showed slower elimination. The AUC(0-∞) was increased by 3.0-fold in liposomes in comparison with standard solution (20 mg·kg-1), the half-life (T1/2) was 1.6- and 1.5-fold higher compared to the reference groups of 20 and 40 mg·kg-1, respectively. Conclusion: Therefore, it could be concluded that liposomal encapsulation effectively improved the bioavailability and pharmacokinetic property of antifungal peptides.

scholarly journals RAPID ANALYTICAL METHOD FOR ASSAY DETERMINATION FOR PROCHLORPERAZINE EDISYLATE DRUG SUBSTANCES BY ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY

2017 ◽  
Vol 9 (4) ◽  
pp. 118 ◽  
Author(s):  
Kishorkumar L. Mule
Keyword(s):  
Liquid Chromatography ◽  
Trifluoroacetic Acid ◽  
Analytical Method ◽  
Mobile Phase ◽  
Ultra Performance Liquid Chromatography ◽  
Drug Substance ◽  
Assay Method ◽  
Column Temperature ◽  
Drug Substances

Objective: To develop and validate new, simple and rapid assay method for Prochlorperazine edisylate drug substance by UPLC as per ICH guidelines.Methods: Ultra performance liquid chromatographic method was developed, optimized and validated on Acquity UPLC by using Acquity BDH300 C4 (100 x 2.1 mm) 1.7µ column. 3.85g ammonium acetate in 1000 ml of water add 0.5 ml trifluoroacetic acid and 1 ml triethylamine (Mobile phase A): 0.5 ml trifluoroacetic acid in 1000 ml acetonitrile mobile phase (Mobile phase B) with gradient program. Detector wavelength 254 nm and column temperature 30 °C.Results: Linearity study was carried out for prochlorperazine edisylate, linearity was calculated from 80 % level to 120% with respect to specification level. The correlation coefficient (r) = 0.999 was proved that the method is robust. The resolution between known impurities and Prochlorperazine edisylate found more than 2.5, it was evident from specificity test that Prochlorperazine edisylate peak are well separated from its related impurities, hence the method is specific. Prochlorperazine edisylate sample solution and mobile phase were found to be stable for at least 3 d.Conclusion: A new, simple and rapid method has been developed and validated for assay determination of prochlorperazine edisylate in drug substance by Ultra Performance Liquid Chromatography (UPLC). The analytical method was developed and validated as per ICH guidelines. The developed method can be used for the fast assay determination of prochlorperazine edisylate drug substances in research laboratories and in the pharmaceutical industry. 

Detection, Quantitation, and Identification of Residual Aminopenicillins by High-Performance Liquid Chromatography after Fluorescamine Derivation

2000 ◽  
Vol 63 (10) ◽  
pp. 1421-1425 ◽  
Author(s):  
CHIH-CHUN HONG ◽  
FUSAO KONDO
Keyword(s):  
Bovine Serum ◽  
Mobile Phase ◽  
High Performance ◽  
Serum Proteins ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Excitation Wavelength ◽  
Column Temperature ◽  
Solid Phase Extraction Cartridge ◽  
Mobile Phases

A high-performance liquid chromatographic (HPLC) method with fluorescence detection after precolumn fluorescamine derivation was developed to detect residues of two aminopenicillins, amoxicillin (AMPC) and ampicillin (ABPC), in bovine serum. Proteins in serum samples spiked with each of these penicillins were precipitated with sodium tungstate and sulfuric acid, centrifuged, and removed by passage through a C18 solid-phase extraction cartridge. After precolumn treatment of the extraction products of AMPC and ABPC with fluorescamine solution, HPLC analysis with fluorescence spectrophotometric detection at an excitation wavelength of 390 nm and an emission wavelength of 485 nm was performed to identify these products. Two mobile phases were used for residual analysis by the isocratic HPLC system. An ODP column (polyvinyl alcohol bonded with an octadecyl functional group) that can be used with strongly alkaline mobile phases (pH 2.0 to 13) was selected, and the column temperature was set at 40°C. A mobile phase comprising 100-mM K2HPO4 solution and acetonitrile (72:28, vol/vol), which yielded AMPC and ABPC retention times of 4.1 and 7.9 min, respectively, was suitable for detection of residual ABPC but not for residual AMPC because interference was caused by peaks of other extracted substances. When a mobile phase comprising a different ratio of 100-mM K2HPO4 solution and acetonitrile (78:22, vol/vol) was used, the retention times of AMPC and ABPC were 7.3 and 26.3 min, respectively, and both penicillins could be analyzed using this system. The calculated standard curves of the reaction products with both mobile phases were linear, and the correlation coefficients were greater than 0.999. The lower limit of detection was 10 ng/ml for both penicillins. Analysis of extracts from bovine serum spiked with AMPC and ABPC at a concentration of 1 μg/ml yielded recovery rates of 102.2 ± 5.5% and 79.0 ± 5.2%, respectively. This detection method may be useful for routine laboratory testing of AMPC and ABPC.

scholarly journals DETERMINATION OF 2-CYANO-4’-BROMOMETHYL BIPHENYL GENOTOXIC IMPURITY IN IRBESARTAN DRUG SUBSTANCES USING HPLC TECHNIQUE

2016 ◽  
Vol 8 (12) ◽  
pp. 225
Author(s):  
S. Senthil Kumar ◽  
Ritesh Kumar Srivastava ◽  
V. Srinivas Rao
Keyword(s):  
Mobile Phase ◽  
Hplc Method ◽  
Development Activity ◽  
Validation Data ◽  
Column Temperature ◽  
Injection Volume ◽  
Drug Substances ◽  
Hplc Technique ◽  
Ich Guideline

<p><strong>Objective: </strong>The objective of present study was to develop and validate a specific and sensitive HPLC method for the quantitative determination of genotoxic impurity 2-cyano-4’-bromomethyl biphenyl present in irbesartan drug substance.</p><p><strong>Methods: </strong>The development activity was conducted by HPLC with UV as a detector. The impurity was separated on Kromasil C18 250 x 4.6 mm, 5 µm analytical column with a mobile phase consisting of buffer pH 3.2 and acetonitrile in the ratio of 60:40 v/v at a flow rate 1.5 ml/min. The effluent was monitored by UV detection at 258 nm with column temperature maintained at 40 °C and the injection volume 30 μl. Acetonitrile was selected as diluent.</p><p><strong>Results: </strong>Validation activity was planned and completed based on the ICH guideline. The LOD and LOQ value were found to be 0.167 µg/g and 0.506 µg/g and accuracy results were well in the range 98.34 to 103.46 %. The linearity curve showed the correlation coefficient of 0.9999 and method very sensitive.</p><p><strong>Conclusion: </strong>From validation data, it was confirmed that the developed method is specific, sensitive, linear, precise and accurate for the determination of 2-cyano-4’-bromomethyl biphenyl genotoxic impurity in irbesartan drug substances.</p>

scholarly journals SIMPLE AND RAPID METHOD FOR THE SIMULTANEOUS ANALYSIS OF TAMOXIFEN, ENDOXIFEN, AND 4-HYDROXYTAMOXIFEN IN DRIED BLOOD SPOT USING LIQUID CHROMATOGRAPHY–TANDEM MASS SPECTROMETRY

2020 ◽  
pp. 112-120
Author(s):  
BAITHA PALANGGATAN MAGGADANI ◽  
YAHDIANA HARAHAP ◽  
HARMITA ◽  
SAMUEL J. HARYONO ◽  
TESANIKA RIBKA JOULIN SITORUS
Keyword(s):  
Formic Acid ◽  
Mobile Phase ◽  
Internal Standard ◽  
Cancer Recurrence ◽  
Dried Blood Spot ◽  
Active Metabolites ◽  
Drying Time ◽  
Liquid Chromatography Tandem Mass ◽  
Blood Spot ◽  
Spot Volume

Objective: Tamoxifen (TAM) is a hormonal therapy that is clinically proven to reduce breast cancer recurrence by blocking estrogen receptor, mainly through its active metabolites, 4-hydroxytamoxifen (4HT) and endoxifen (END), which have a higher affinity to ER than TAM itself. The objective of the present study was to develop and validate simple and rapid LC-MS/MS method for analysis TAM and its metabolites simultaneously in dried blood spot (DBS) sample for monitoring studies purposes. Methods: Optimization was done by evaluating several parameters that affect the efficiency of DBS preparation, such as blood spot volume, drying time and extraction method from the DBS paper. The effectiveness of chromatographic conditions was also optimized by varying flow rate, mobile phase combination and gradient. Clomiphene was used as the internal standard. Results: The result showed that preparation of 20 µl blood spot volume with 120 min of drying time and 25 min of extraction time using 1 ml methanol was the most efficient condition and also fulfilled recovery and matrix effect requirement according to FDA and EMA guidelines. The separation was performed on UPLC Class BEH C18 using formic acid 0.1%-formic acid 0.1% in acetonitrile (35:65) as the mobile phase in isocratic mode at 0.25 ml/min with a total analysis time of 4 min. Conclusion: This method has successfully fulfilled all validation requirements referring to EMA and FDA guidelines.

scholarly journals ISOLATION, CHARACTERIZATION AND VALIDATION OF HPLC METHOD FOR QUANTIFICATION OF BIS-[10-(2-METHYL-4H-3-THIA-4,9-DIAZABENZO[F]AZULENE)]-1,4-PIPERAZINE IN AN ANTI-PSYCHOTIC DRUG SUBSTANCE, OLANZAPINE

2018 ◽  
Vol 10 (4) ◽  
pp. 22
Author(s):  
Suresh Babu Bodempudi ◽  
Ravi Chandra Babu Rupakula ◽  
Konda S. Reddy ◽  
Mahesh Reddy Ghanta
Keyword(s):  
Mobile Phase ◽  
Sodium Hydroxide Solution ◽  
Linear Regression Analysis ◽  
Sodium Dodecyl ◽  
Hplc Method ◽  
Drug Substance ◽  
Phase System ◽  
Column Temperature ◽  
Relative Standard

Objective: The main objective of present study was to Isolate, characterize and validate a reverse phase high performance liquid chromatographic method was validated for quantification of bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine in Olanzapine drug substance; it decreases the mental disorders in human body. The method is specific, rapid, precise and accurate for the separation and determination of bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine in Olanzapine drug substance form.Methods: The bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine of Olanzapine was resolved on a Zorbax RX-C 8, 250 mm X 4.6 mm, 5 micron column (L-1) using a mobile phase system containing 0.03 M sodium dodecyl sulphate in water pH 2.5 with 1 N sodium hydroxide solution and acetonitrile in the ratio of (Mobile phase A-52:48 v/v) and (Mobile phase B-buffer and Acetonitrile 30:70 v/v) by using the gradient program. The mobile phase was set at a flow rate of 1.5 ml/min and the volume injected was 20μl for every injection. The detection wavelength was set at 220 nm and the column temperature was set at 35 °C.Results: The proposed method was productively applied for the quantitative determination of bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo [f]azulene)]-1,4-piperazine in Olanzapine drug substance form. The linear regression analysis data for calibration plots showed a good linear relationship over a concentration range of 0.025to 0.903 µg/ml for bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine, 0.081-0.608 µg/ml for Olanzapine. The mean values of the correlation coefficient were 0.999 and 0.999 for bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine and Olanzapine. The method was validated as per the ICH guidelines. The detection limit (LOD) was about 0.007 µg/ml, 0.024 µg/ml and quantitation limit (LOQ) was about 0.024 µg/ml, 0.081 µg/ml for bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine and Olanzapine. The relative standard deviation was found to be 1.64 % and 2.18 % for bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine and Olanzapine.Conclusion: The validated HPLC method and the statistical analysis showed that the method is repeatable and selective for the estimation of the bis-[10-(2-methyl-4H-3-thia-4,9-diazabenzo[f]azulene)]-1,4-piperazine of the Olanzapine drug substance.

scholarly journals Determination of Nitroimidazole Residues in Porcine Urine by Liquid Chromatography/TandemMass Spectrometry

2006 ◽  
Vol 89 (4) ◽  
pp. 1116-1119 ◽  
Author(s):  
Xi Xia ◽  
Xiaowei Li ◽  
Jianzhong Shen ◽  
Suxia Zhang ◽  
Shuangyang Ding ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
Solid Phase ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Mass Spectrometry System ◽  
Ionization Mode ◽  
Positive Ion ◽  
Mode A

Abstract A reliable and sensitive method was developed for determination of nitroimidazoles in porcine urine. Sample preparation involves an extraction with ethyl acetate, followed by a solid-phase extraction cleanup step. The final extract is injected into the liquid chromatography/tandem mass spectrometry system in the positive-ion electrospray ionization mode. A C8 column with water and acetonitrile as the mobile phase is used for chromatographic separation under gradient conditions. Overall average recoveries ranged from 83 to 107%. The limits of detection ranged from 0.03 to 0.05 ng/mL, and the limits of quantitation, from 0.1 to 0.2 ng/mL.

scholarly journals An HPLC method for the determination of digoxin in dissolution samples

2010 ◽  
Vol 75 (11) ◽  
pp. 1583-1594 ◽  
Author(s):  
Miroslav Milenkovic ◽  
Valentina Marinkovic ◽  
Predrag Sibinovic ◽  
Radosav Palic ◽  
Dragan Milenovic
Keyword(s):  
Mobile Phase ◽  
Hplc Method ◽  
Stability Testing ◽  
Column Length ◽  
Column Temperature ◽  
Chromatographic Parameters ◽  
The Impact ◽  
Full Factorial ◽  
Phase Column

An HPLC method for digoxin quantification in dissolution samples obtained as per the official British Pharmacopeia (BP) method is presented in this paper. The chromatography was performed at 20 ?C on a Symmetry C18; 3.5 ?m, 75 x 4.6 mm column with water - acetonitrile (72 : 28, v/v), as the mobile phase and UV detection at 220 nm. The method was found to be selective, linear, accurate and precise in the specified ranges. The LOD and LOQ were 0.015 ?g mL-1 and 0.050 ?g mL-1, respectively. Robustness testing was conducted to evaluate the impact of minor changes in the chromatographic parameters (i.e., acetonitrile fraction, flow rate of the mobile phase, column temperature and column length) on the characteristics of the digoxin peak. A. full factorial design (24) was used to investigate the influence of the four variables The presented HPLC method was applied in quality and stability testing of Digoxin tablets 0.25 mg.

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