Simple GC-FID method development and validation for determination of α-tocopherol (vitamin E) in human plasma

2007 ◽  
Vol 70 (3) ◽  
pp. 363-368 ◽  
Author(s):  
Fatma Demirkaya ◽  
Yucel Kadioglu
Keyword(s):  
Vitamin E ◽  
Human Plasma ◽  
Method Development ◽  
Method Development And Validation ◽  
Development And Validation

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 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

SENSITIVE BIO ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF VENETOCLAX IN HUMAN PLASMA BY LC-ESI-MS/MS

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (06) ◽  
pp. 32-38
Author(s):  
H. Potluri ◽  
Keyword(s):  
Human Plasma ◽  
Method Development ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Liquid Liquid Extraction ◽  
Liquid Chromatography Tandem Mass ◽  
Positive Mode ◽  
Method Development And Validation ◽  
Development And Validation

A specific and sensitive method of liquid chromatography–tandem mass spectrometry was demonstrated for the experimental determination of venetoclax in human plasma utilising venetoclax-D8 as an internal standard. The column Xbridge C18, 50 × 4.6mm, 5 µm was used for attaining chromatographic separation by utilising 10mM ammonium formate and methanol as isocratic mobile phase in the composition ratio of 20:80 (V/V). The flow-rate selected was 0.7ml/min. Venetoclax and venetoclax-D8 are identified in multiple reaction monitoring (MRM) positive mode with proton adducts at m/z 869.53 →553.21 and m/z 877.14 → 553.23, respectively. For the successful extraction of drug as well as internal standard, liquid-liquid extraction technique was efficiently utilised. The developed technique was established in a linear concentration range of 5.0-5000.0 pg/ml along with correlation coefficient (r2) of 0.9994. Intra and inter-day precisions were found to be 0.7 to 1.90% and 0.7 to 2.0 % for venetoclax and venetoclax-D8, respectively. Accuracy was found to be within 98.6 to 101.99% and 99.17 to 101.14 % for venetoclax and venetoclax-D8, respectively. It was observed that throughout the bench top studies, post-operative stability studies and freeze-thawing cycles, venetoclax retained stability.

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 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.

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