scholarly journals Bioanalytical Method Development and Validation for the Simultaneous Determination of Vildagliptin and Telmisartan in Rabbit Plasma Using RP-HPLC

2021 ◽  
pp. 76-86
Author(s):  
Budideti Kishore Kumar Reddy ◽  
Kothapalli Bonnoth Chandra Sekhar ◽  
Chinnala Krishna Mohan
Keyword(s):  
Simultaneous Determination ◽  
Method Development ◽  
Extraction Procedure ◽  
Methyl Tert Butyl Ether ◽  
Isosbestic Point ◽  
Therapeutic Drug ◽  
Rabbit Plasma ◽  
Butyl Ether ◽  
Bioanalytical Method

A simple, reproducible bioanalytical method of liquid chromatography and PDA detector was developed and validated for the simultaneous Determination of Vildagliptin and Telmisartan in Rabbit Plasma using liquid-liquid extraction technique. K2 EDTA was used as anti-coagulant. Analytes were extracted by Methyl-tert-Butyl Ether (MTBE) and subsequent separation on a Kromasil C18 column (5 µ, 100 × 4.6 mm) using Acetonitrile : Methanol 75:25 v/v as mobile phase at a flow rate of 1 mL/min and (40±1)°C column oven temperature. Analytes were monitored with PDA detector at an isosbestic point of 225 nm for both Vildagliptin and Telmisartan.  Retention times of Vildagliptin and Telmisartan were found to be at 2.545 mins and 6.633 mins respectively. The method was validated over a linear (r2 = 0.9979) concentration range of 24.979 - 5003.808  µg/ml for Vildagliptin and 1.011- 202.559 µg/ml for Telmisartan. The inter-day and intra-day precisions were found to be less than 15% and the accuracy was all within ±15% (at LLOQ ±20%). The developed HPLC-PDA method was fully validated for all the other parameters as per FDA guidelines like selectivity, matrix effect, recovery and stability as well. Due to the high degree of sensitivity, very less time consuming, easy extraction procedure and low requirement of sample volume, the method will be applicable for therapeutic drug monitoring.

scholarly journals Development and validation of LC–MS/MS method for determination of DNDI-VL-2098 in mouse, rat, dog and hamster blood

Bioanalysis ◽  
2019 ◽  
Vol 11 (15) ◽  
pp. 1419-1435
Author(s):  
Bhavesh D Patel ◽  
Ritika Uppal ◽  
Nageswararao Pulakundam ◽  
Jignesh P Patel ◽  
Vikram Ramanathan ◽  
...  
Keyword(s):  
Dynamic Range ◽  
Extraction Procedure ◽  
Methyl Tert Butyl Ether ◽  
Butyl Ether ◽  
Bioanalytical Method ◽  
Liquid Liquid Extraction ◽  
Fit For Purpose ◽  
Dog Blood ◽  
Development And Validation

Aim: To develop a bioanalytical method to support pharmacokinetic evaluation of DNDI-VL-2098 in mouse, rat, dog and hamster following oral administration. Results & methodology: A robust LC–MS/MS bioanalytical method was developed to quantify DNDI-VL-2098. DNDI-VL-2098 showed time-dependent recovery loss in acetonitrile precipitated plasma in all species. Acid-lysed whole blood was identified as a matrix in which recovery was stable over time. A two-step extraction procedure was used, with protein precipitation followed by liquid–liquid extraction with methyl tert-butyl ether. The assay was validated in the dynamic range of 5–5000 ng/ml for mouse, rat and dog blood, and a fit-for-purpose method was developed for hamster. Conclusion: A specific LC–MS/MS assay for DNDI-VL-2098 was developed and validated in hemolyzed blood.

scholarly journals Bioanalytical Method Development and Validation for Determination of Sulfasalazine in Rabbit Plasma by HPLC-UV

2021 ◽  
Vol 33 (7) ◽  
pp. 1692-1698
Author(s):  
S.S. Jadiya ◽  
N. Upmanyu ◽  
S. Arulmozhi ◽  
V. Jain ◽  
S. Sankaran ◽  
...  
Keyword(s):  
High Performance ◽  
Method Development ◽  
High Efficiency ◽  
Internal Standard ◽  
Ultra Violet ◽  
Precipitation Method ◽  
Pharmacokinetic Studies ◽  
Rabbit Plasma ◽  
Bioanalytical Method

In present study, an advanced, simple and a rapid reverse phase high performance liquid chromatography (RP-HPLC) method was developed for the quantitative determination of sulfasalazine in rabbit plasma. Sulfasalazine was separated using Chromatopak C-18 basic peerless (250 mm × 4.6 mm, 5μ) column in an isocratic mode using mobile phase consisting of the mixture of 10mM Ammonium acetate pH adjusted to 4.5 and acetonitrile (70:30 v/v) with a flow rate of about 1.0 mL/min at ambient temperature. An ultra-violet detection of sulfasalazine and the internal standard was carried out at 362 nm. Both sulfasalazine and internal standard (IS, 4-hydroxy benzoate) were extracted from plasma matrices with high efficiency using a simple protein precipitation method. The method was found to be highly selective with no carryover effects. Linearity of sulfasalazine was found with the range of 2.5-100 μg/mL with the value of r2 > 0.995 a correlation coefficient. At all three quality control levels, developed bioanalytical method was found as repeatable and reproducible as well. The average recoveries of sulfasalazine from plasma were in the range of 95.59-97.16%. The bioanalytical samples showed good and acceptable stability of sulfasalazine solution at different storage, packaging and handling conditions. Hence, in conclusion, the validated and developed HPLC-UV method could be effectively utilized for determination of sulfasalazine in pharmacokinetic studies involving novel formulations.

Dual design spaces for micro-extraction together with the core–shell chromatographic determination of dorzolamide and timolol in rabbit plasma: an example of quality by design method development

2016 ◽  
Vol 40 (10) ◽  
pp. 8424-8437 ◽  
Author(s):  
Abdel-Maaboud Ismail Mohamed ◽  
Hanaa Mohammed Abdel-Wadood ◽  
Heba Salah Mousa
Keyword(s):  
Simultaneous Determination ◽  
Chromatographic Method ◽  
Method Development ◽  
Quality By Design ◽  
Design Method ◽  
Chromatographic Determination ◽  
Core Shell ◽  
Rabbit Plasma ◽  
The Core

An innovative quality by design-integrated VA-SALLME-core–shell chromatographic method was developed for the simultaneous determination of DOR and TIM in plasma.

scholarly journals Simultaneous Determination of Carotenoids and Chlorophylls by the HPLC-UV-VIS Method in Soybean Seeds

Agronomy ◽  
2021 ◽  
Vol 11 (4) ◽  
pp. 758
Author(s):  
Berhane Sibhatu Gebregziabher ◽  
Shengrui Zhang ◽  
Jie Qi ◽  
Muhammad Azam ◽  
Suprio Ghosh ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Reversed Phase ◽  
Methyl Tert Butyl Ether ◽  
Coefficient Of Determination ◽  
Detector Response ◽  
Soybean Seeds ◽  
Butyl Ether ◽  
Legume Seeds ◽  
Relative Standard

Soybean contains nutritional bioactive compounds, including carotenoids associated with human health benefits. Carotenoids are applicable in pharmaceuticals/nutreceuticals, cosmetic, and mainly food industries. However, an efficient and accurate method for carotenoid and chlorophyll detection and quantification has not yet been developed and validated for soybean seeds. The need for a rapid and reliable analysis method has become increasingly important. Thus, this study was initiated to develop and validate a simple, rapid, and selective reversed-phase high-performance liquid chromatographic (RP-HPLC) method for the simultaneous determination of lutein, zeaxanthin, α-carotene, β–carotene, β–cryptoxanthin, and chlorophyll–a and –b in soybean flour sample (100.00 mg) extracted using ethanol-acetone (1:1) solvents at a volume of 1.50 mL. Interestingly, the effective separation technique was achieved using the mobile phases of methyl tert-butyl ether, methanol containing 10 mM ammonium acetate, and water delivered at a 0.90 mL min−1 flow rate through a C30YMC Carotenoid (250 × 4.6 mm I.D., S-5 µm) column coupled with a UV-VIS detector set at 450 nm. The detector response was linear from 0.05–30.00 μg mL−1 with a coefficient of determination (R2) of 0.9993–0.9999. The validated method was sensitive with a detection limit (LOD) of 0.0051–0.0300 μg mL−1 and 0.0155–0.0909 μg mL−1 for the quantification limit (LOQ). The recovery values were from 83.12–106.58%, and the repeatability precision ranged from 1.25–4.20% and 0.15–0.81% for the method and system, respectively. The method showed adequate precision with a relative standard deviation smaller than 3.00%. This method was also found to be applicable for profiling carotenoids and chlorophylls in other legumes. In summary, this method was successfully implemented for qualitative and quantitative determination of major carotenoids and chlorophylls in soybean and other legume seeds, which are beneficial to food industry and quality breeding programs to meet human nutrition demands globally.

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