scholarly journals LC-MS/MS Method Development and Validation for the Determination of Nifedipine in Human Plasma

2020 ◽  
Vol 10 (5) ◽  
pp. 6189-6196
Keyword(s):  
Human Plasma ◽  
Method Development ◽  
Accurate Method ◽  
Routine Examination ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
The Mean ◽  
Development And Validation ◽  
Gradient Mode

The main purpose of this study was to develop a simple, precise, rapid, green and accurate method for the simultaneous quantification of nifedipine in human plasma; The resolution of peaks was best achieved with Intersil ODS gum C18 (4.6 × 50 mm, 3.5 μm) column. Samples were chromatographed in a gradient mode (acetonitrile – water – formic acid). The mobile phase was delivered at a flow rate of 0.500 mL/min into the mass spectrometer ESI chamber; The total chromatographic run time was 4 minutes. Nifedipine eluted at ~3.24 min. A linear response function was established at 1 - 130 ng/mL in human plasma. The % mean recovery in LQC, MQC and HQC was 104.1 %, 105.0 % and 108.7 %. The lowest concentration with the RSD <20% was taken as LLOQ and was found to be 1.01 ng/mL. The % accuracy of LLOQ samples prepared with the different biological matrix lots was found 100.5 % for nifedipine, which was found within the range of 80.00-120.00 % for the seven different plasma lots. A rapid method was developed for the determination of nifedipine in human plasma. The method was strictly validated according to the ICH guidelines. Acquired results demonstrate that proposed strategy can be effortlessly and advantageously applied for routine examination of nifedipine in human plasma.

scholarly journals LC-MS/MS METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF CARDIAZOL IN HUMAN PLASMA

2019 ◽  
pp. 380-385
Author(s):  
IRYNA DRAPAK ◽  
BORYS ZIMENKOVSKY ◽  
LINA PEREKHODA ◽  
SERGIY KOVALENKO ◽  
Liliya Logoyda
Keyword(s):  
Formic Acid ◽  
Human Plasma ◽  
Method Development ◽  
Accurate Method ◽  
Sample Volume ◽  
Ich Guidelines ◽  
Coefficients Of Variation ◽  
Method Development And Validation ◽  
Development And Validation

Objective: The main purpose of this study was to develop a simple, precise, rapid and accurate method for the quantification of cardiazol in human plasma. Methods: Chromatography was achieved on Discovery C18, 50 × 2.1 mm, 5 μm column. Samples were chromatographed in a gradient mode (eluent A (acetonitrile-water–formic acid, 5: 95: 0.1 v/v), eluent B (acetonitrile–formic acid, 100: 0.1 v/v)). The initial content of the eluent B of 8%, which increases linearly to 1.0 min to 100%, is maintained up to 1.5 min and returned to the original 8% to 1.51 min. The mobile phase was delivered at a flow rate of 0.400 ml/min into the mass spectrometer ESI chamber. The sample volume was 300 μl. Results: The total chromatographic run time was 2.5 min and the elution of cardiazol and IS (difenoconazole) occurred at ~2.15 and 1.98 min, respectively. A linear response function was established at 1-100 ng/ml for cardiazol and difenoconazole in human plasma. The % mean recovery for cardiazol in LQC, MQC and HQC was 102.8 %, 100.3 % and 95.9 %. The lowest concentration with the RSD<20% was taken as LLOQ and was found to be 1.10 ng/ml for cardiazol. The % accuracy of LLOQ samples prepared with the different biological matrix lots was found 109.7 %, which were found within the range of 80.00-120.00 % for the seven different plasma lots. % CV for LLOQ samples was observed as 11.9 %, which are within 20.00% of the acceptance criteria. The within-run coefficients of variation ranged between 0.311 % and 0.601 % for cardiazol. The within-run percentages of nominal concentrations ranged between 99.80 % and 100.41 % for cardiazol. The between-run coefficients of variation ranged between 0.332 % and 0.615 % for cardiazol. The between-run percentages of nominal concentrations ranged between 98.18 % and 101.21 % for cardiazol. Conclusion: A rapid method was developed for simultaneous determination of cardiazol in human plasma. The method was strictly validated according to the ICH guidelines. Acquired results demonstrate that the proposed strategy can be effortlessly and advantageously applied for routine examination of cardiazol in human plasma.

scholarly journals Bioanalytical method development and validation for the determination of metoprolol and meldonium in human plasma

Pharmacia ◽  
2020 ◽  
Vol 67 (2) ◽  
pp. 39-48
Author(s):  
Mariana Horyn ◽  
Liliya Logoyda
Keyword(s):  
Formic Acid ◽  
Human Plasma ◽  
Mobile Phase ◽  
Method Development ◽  
Accurate Method ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Phase Water ◽  
Development And Validation

Aim.The main purpose of this study was to develop a simple, precise, rapid and accurate method for the quantification of metoprolol and meldonium in human plasma. Materials and methods. The resolution of peaks of metoprolol was best achieved with Discovery C18, 50 × 2.1 mm, 5 μm column and meldonium - ZORBAX HILIC Plus, 50 × 2.1 mm, 3.5 μm column. Samples of metoprolol were chromatographed in a gradient mode (eluent A (acetonitrile – water – formic acid, 5 : 95 : 0.1 v/v), eluent B (acetonitrile – formic acid, 100 : 0.1 v/v)). The initial content of the eluent B is 0%, which increases linearly by 1.0 min to 100% and to 1.11 min returns to the initial 0%. The mobile phase was delivered at a flow rate of 0.400 mL/min into the mass spectrometer ESI chamber. The injection volume was 5μl. Samples of meldonium were chromatographed in a isocratic using mobile phase water – acetonitrile – ammonium formate buffer 200 мМ, 20 : 75 : 5 v/v). Results.The total chromatographic run time was 2.0 minutes and the elution of metoprolol, meldonium and IS occurred at ~1.39 and 1.18 minutes, respectively.A linear response function was established at 2 - 200 ng/mL for metoprolol and 50 -5000 ng/mL for meldonium in human plasma. The% mean recovery for metoprolol in LQC, MQC and HQC was 99.0%, 107.5% and 96.8%, for meldonium in LQC, MQC and HQC was 94.1%, 100.2% and 93.1% respectively. The lowest concentration with the RSD &lt;20% was taken as LLOQ and was found to be 2.31 ng/mL for metoprolol, 47.70 ng/mL for meldonium. The % accuracy of LLOQ samples prepared with the different biological matrix lots were found 115.4% for metoprolol and 95.5% for meldonium, which were found within the range of 80.00–120.00% for the seven different plasma lots. % CV for LLOQ samples was observed as 12.8% and 7.7% respectively, which are within 20.00% of the acceptance criteria. Conclusion.A rapid method was developed for simultaneous determination of metoprolol and meldonium in human plasma. The method was strictly validated according to the ICH guidelines. Acquired results demonstrate that proposed strategy can be effortlessly and advantageously applied for routine examination of metoprolol and meldonium in human plasma.

scholarly journals A HPLC-MS/MS METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS DETERMINATION OF NIFEDIPINE AND ENALAPRIL IN HUMAN PLASMA

2018 ◽  
Vol 10 (4) ◽  
pp. 35 ◽  
Author(s):  
Liliya Logoyda
Keyword(s):  
Formic Acid ◽  
Simultaneous Determination ◽  
Human Plasma ◽  
Method Development ◽  
Accurate Method ◽  
Sample Volume ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Development And Validation

Objective: The main purpose of this study was to develop a simple, precise, rapid and accurate method for the simultaneous quantification of nifedipine and enalapril in human plasma.Methods: Chromatography was achieved on Discovery C18, 50 × 2.1 mm, 5 μm column. Samples were chromatographed in a gradient mode (eluent A (acetonitrile-water–formic acid, 5: 95: 0.1 v/v), eluent B (acetonitrile–formic acid, 100: 0.1 v/v)). The initial content of the eluent B is 0%, which increases linearly by 1.0 min to 100% and to 1.01 min returns to the initial 0%. The mobile phase was delivered at a flow rate of 0.400 ml/min into the mass spectrometer ESI chamber. The sample volume was 5 μl.Results: The total chromatographic run time was 2.5 min and the elution of nifedipine, enalapril and IS (verapamil) occurred at ~1.83, 1.57 and 1.61 min, respectively. A linear response function was established at 1-100 ng/ml for nifedipine and 2-200 ng/ml for enalapril maleate in human plasma. The % mean recovery for enalapril in LQC, MQC and HQC was 114.0 %, 112.9 % and 113.2 %, for nifedipine in LQC, MQC and HQC was 104.1 %, 105.0 % and 108.7 % respectively. The lowest concentration with the RSD<20% was taken as LLOQ and was found to be 2.16 ng/ml for enalapril, 1.01 ng/ml for nifedipine. The % accuracy of LLOQ samples prepared with the different biological matrix lots was found 108.2 % for enalapril and 100.5 % for nifedipine, which were found within the range of 80.00-120.00 % for the seven different plasma lots. % CV for LLOQ samples was observed as 3.2 % and 7.4 % respectively, which are within 20.00% of the acceptance criteria.Conclusion: A rapid method was developed for simultaneous determination of nifedipine and enalapril in human plasma. The method was strictly validated according to the ICH guidelines. Acquired results demonstrate that proposed strategy can be effortlessly and advantageously applied for routine examination of nifedipine and enalapril in human plasma. 

scholarly journals Stability indicating RP-HPLC method development and validation for the simultaneous estimation of ceftriaxone and tazobactum in sterile powder for injection

2019 ◽  
Vol 1 (2) ◽  
pp. 40-43
Author(s):  
T. Vimalakkannan ◽  
P. Shaik Parveen ◽  
Salomi ◽  
K. Ravindra Reddy
Keyword(s):  
Method Development ◽  
Pharmaceutical Formulations ◽  
Accurate Method ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Hplc Method Development ◽  
Development And Validation

A simple, rapid, precise and accurate method is developed for the quantitative simultaneous determination of ceftriaxone and tazobactum in bulk and pharmaceutical formulations. Separation of ceftriaxone and tazobactum was successfully achieved by using Inertsil C18 ODS column 250X4.6mm, 5µm in an isocratic mode using water and acetonitrile (80:20) at a flow rate of 1.0 ml/min and was monitored at 254 nm with a retention time of 3.049 minutes and 4.317 minutes for ceftriaxone and tazobactum respectively. The method was validated and the response was found to be linear in the drug concentration range of 20µg/ml to 80 µg/ml for ceftriaxone and 5 µg/ml to 35 µg/ml for tazobactum. The values of the correlation coefficient were found to be 0.999 for ceftriaxone and 0.999 for tazobactum respectively. The LOD and LOQ for ceftriaxone were found to be 0.021 and 0.064 respectively. The LOD and LOQ for tazobactum were found to be 0.030 and 0.091 respectively. The percentage recovery for ceftriaxone and tazobactum were found to be 98-102% respectively which indicates that the proposed method is highly accurate. The specificity of the method shows good correlation between retention times of standard with the sample. The method was extensively validated according to ICH guidelines for Linearity, Accuracy, Precision, Specificity and Robustness.  Stability of the drugs was determined by using acid/base, thermal, oxidative stress testing.

scholarly journals Bioanalytical Method Development and Validation of Estimation of Nimorazole by RP-HPLC in Human Plasma

2019 ◽  
Vol 12 (4) ◽  
pp. 7-12
Author(s):  
Nilam B Jadhav ◽  
Savita S Yadav ◽  
Kuldeep Singh Gusain
Keyword(s):  
Human Plasma ◽  
Method Development ◽  
Therapeutic Drug ◽  
Main Principle ◽  
Liquid Liquid Extraction ◽  
Rp Hplc ◽  
Method Development And Validation ◽  
The Mean ◽  
Development And Validation

Nimorazole is an antiprotozoal medicine used to treat infections caused by protozoa in the stomach, intestines, or genital areas. The main principle of this study was to develop RP-HPLC technique for the quantitative determination of Nimorazole in human plasma. The separation was accomplished by the isocratic method by using column C18 (Thermosil ODS), detection wavelength was 294 nm. The analyte was extracted in acetonitrile by liquid-liquid extraction. Acetonitrile: water in the ratio 30:70 was used as mobile phase for estimation of the drug in human plasma with a flow rate of 0.8 mL/min at a detection wavelength of 294 nm. Retention time was found to be 7.933 ± 0.23 min.The developed method was found to be linear over the concentration range of 60-360 μg/mL, with a correlation coefficient of 0.9991. The LOD and LOQ were found to be 10 μg/mL and 40 μg/mL, respectively. The method ensure for Precision and % RSD was found to be less than 2 % and the mean % recovery was found to be 99.58%. This method was effectively and favourably applied to the plasma samples and it seems to be appropriate tool for regular therapeutic drug monitoring of anti-infective drugs.

scholarly journals A HPLC-MS/MS METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS DETERMINATION OF BISOPROLOL AND ENALAPRIL IN THE PRESENT OF ENALAPRILAT IN HUMAN PLASMA

2018 ◽  
Vol 10 (2) ◽  
pp. 31 ◽  
Author(s):  
Liliya Logoyda ◽  
Dmytro Korobko ◽  
Oleksandra Oleshchuk ◽  
Taras Proniv ◽  
Mariya Dmutriv
Keyword(s):  
Formic Acid ◽  
Simultaneous Determination ◽  
Human Plasma ◽  
Method Development ◽  
Sample Volume ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Initial Content ◽  
Development And Validation

Objective: A highly specific, sensitive and rapid HPLC-MS/MS method has been developed and validated for the simultaneous quantification of bisoprolol and enalapril in the present of enalaprilat in human plasma.Methods: Analytes were extracted from plasma using a protein precipitation extraction method. Chromatography was achieved on Discovery C18, 50 × 2.1 mm, 5 μm column. Samples were chromatographed in a gradient mode (eluent A (acetonitrile-water–formic acid, 5: 95: 0.1 v/v), eluent B (acetonitrile–formic acid, 100: 0.1 v/v)). The initial content of the eluent B is 0%, which increases linearly by 1.0 min to 100% and to 1.01 min returns to the initial 0%. The mobile phase was delivered at a flow rate of 0.400 ml/min into the mass spectrometer ESI chamber. The sample volume was 5 μl.Results: The total chromatographic run time was 2.0 min and the elution of bisoprolol, enalapril, enalaprilat and IS (verapamil) occurred at ~1.01, 1.03, 0.96 and 1.09 min, respectively. A linear response function was established at 0.5-50 ng/ml for bisoprolol fumarate, 2-200 ng/ml for enalapril maleate, 1-100 ng/ml for enalaprilat dehydrate in human plasma. The intraday and interday accuracy and precisions were in the range of 0.311 %-0.647 % and 0.364 %-0.572 % for bisoprolol, 0.321 %-0.747 % and 0.390 %-0.673 % for enalapril, 0.221 %-0.547 % and 0.264 %-0.773 % for enalaprilat, respectively.Conclusion: A new rapid method was developed for simultaneous determination of bisoprolol and enalapril in the present of enalaprilat in human plasma. The method was strictly validated according to the ICH guidelines. The information thus obtained from the study can be used for the full pharmacokinetic profiling in individuals. 

scholarly journals Method Development and Validation for the Determination of Pravastatin in Human Plasma by Lc-Ms/Ms

2017 ◽  
Vol 2 (1) ◽  
pp. 1-7
Author(s):  
Lian Chen ◽  
Paresh Joshi ◽  
Andrii Piatkivskyi ◽  
Kalem Aguilar ◽  
Jenny Lin
Keyword(s):  
Human Plasma ◽  
Method Development ◽  
Method Development And Validation ◽  
Development And Validation

scholarly journals Determination of Chromones in Dysophylla stellata by HPLC: Method Development, Validation and Comparison of Different Extraction Methods

2010 ◽  
Vol 5 (4) ◽  
pp. 1934578X1000500 ◽  
Author(s):  
Raju Gautam ◽  
Amit Srivastava ◽  
Sanjay M. Jachak
Keyword(s):  
Method Development ◽  
Gradient Elution ◽  
Extraction Methods ◽  
Hplc Method ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Efficient Extraction ◽  
Hplc Method Development ◽  
Development And Validation

An HPLC method with reflux as an efficient extraction method has been developed for quantification of chromones in Dysophylla stellata Benth. Separation was achieved on a C18 column with a mobile phase of 0.5% (v/v) acetic acid in water (A), and ACN (B) under gradient elution at 1 mL/min. Chromones (1 and 2) isolated from D. stellata were used as standards for method development and validation was achieved according to ICH guidelines. Extracts prepared by three different methods [reflux, ultrasonication and accelerated solvent extraction (ASE)] were used for analysis by the validated method. The proposed HPLC method is simple, accurate and selective for the separation and quantification of chromones in D. stellata.

Sign in / Sign up

Export Citation Format

Share Document