scholarly journals Separation Selectivity of Isoniazid and Asetilisoniazid in Human Plasma In-vitro by High Performance Chromatography

2019 ◽  
Vol 17 (2) ◽  
pp. 238
Author(s):  
Novi Yantih ◽  
Yahdiana Harahap ◽  
Wahono Sumaryono ◽  
Rianto Setiabudy ◽  
Lestari Rahayu

Bioanalysis method is needed to pharmacokinetic study of INH as antituberculosis. The main problem is INH structure is similar to that of acetyl isoniazid (AcINH) as its metabolite. Therefore, a selective separation method is needed to separate the INH from its metabolite and matrix. The aim of this study was to test the selectivity of separation method of INH and AcINH in human plasma in-vitro by high performance liquid chromatography (HPLC). The HPLC system used a reversed phase with UV detector and hexane sulphonate as an ion counter. The optimum conditions was obtained by using C18 as stationary phase, hexane sulphonate (pH 2.47)-methanol (65:35) as mobile phase, with flow rate of 1mL/min, and UV detector at wavelength of 265nm. The selectivity of method separation was indicated by a resolution value of ≥ 1.5. The tailing factor for INH and AcINH were 1.297, dan 1.912, respectively. The k values ware ​​less than 10 and N values ​​were greater than 5000 indicate good separation efficiency. The developing of HPLC was a selective for separating of INH and AcINH in human plasma in-vitro.

1994 ◽  
Vol 59 (3) ◽  
pp. 569-574 ◽  
Author(s):  
Josef Královský ◽  
Marta Kalhousová ◽  
Petr Šlosar

The reversed-phase high-performance liquid chromatography of some selected, industrially important aromatic sulfones has been investigated. The chromatographic behaviour of three groups of aromatic sulfones has been studied. The optimum conditions of separation and UV spectra of the sulfones and some of their hydroxy and benzyloxy derivatives are presented. The dependences of capacity factors vs methanol content in mobile phase are mentioned. The results obtained have been applied to the quantitative analysis of different technical-grade samples and isomer mixtures. For all the separation methods mentioned the concentration ranges of linear calibration curves have been determined.


INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (11) ◽  
pp. 46-50
Author(s):  
Z. G Khan ◽  
◽  
S. S. Patil ◽  
P. K. Deshmukh ◽  
P. O. Patil

Novel, isocratic reversed phase high performance liquid chromatography method was developed and validated for the determination of enzalutamide (EZA) in bulk drug and pharmaceutical formulation. Efficient separation was achieved on PrincetonSPHER C18 100A, 5μ (250×4.6 mm) under the isocratic mode of elution using acetonitrile: water (80:20) % V/V as a mobile phase pumped in to the column at flow rate 1.0 mL/min. The effluent was monitored at 237.0 nm using UV detector. EZA was eluted in the given mobile phase at retention time (tR) of 3.2 minutes. The standard calibration curve was linear over the concentration range 10 - 60 μg/mL with correlation coefficient 0.997. The method was validated for accuracy, precision, sensitivity, robustness, ruggedness and all the resulting data treated statistically. The system suitability parameters like retention time, theoretical plates, tailing factor, capacity factor were found within the limit.


2014 ◽  
Vol 52 (1-2) ◽  
pp. 54-60
Author(s):  
O. Rotkaja ◽  
J. Golushko ◽  
K. Kuprevics

Abstract The chromatographic behavior of tegafur and its impurities on a naphthalene Cosmosil piNAP column under reversed-phase high-performance liquid chromatography conditions was examined. A good description of the retention was achieved through the application of statistical weights to the widely used quadratic relationships between the logarithm of the retention factor (log k) and the organic solvent concentration in the mobile phase. Optimum conditions for isocratic separation of the compounds were found with acetonitrile concentration of 10-30% in the mobile phase


2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Arfana Mallah ◽  
Amber R. Solangi ◽  
Najma Memon ◽  
Rabia A. Memon ◽  
Muhammad Y. Khuhawar

This paper reports the utilization of 2-pyrrolecarboxaldehyde-4-phenylsemicarbazone (PPS) as a complexing reagent for the simultaneous determination and separation of Ni(II), Cu(II), Pd(II), and Ag(I) by reversed-phase high-performance liquid chromatography with UV detector. A good separation was achieved using Microsorb C18 column (150 × 4.6 mm i.d.) with a mobile phase consisted of methanol : acetonitrile : water : sodium acetate (1 mM) (68 : 6.5 : 25 : 0.5 v/v/v/v) at a flow rate of 1 mL/min. The detection was performed at 280 nm. The linear calibration range was 2–10 μg/mL for all metal ions. The detection limits (S/N = 3) were 80 pg/mL for Ni(II), 0.8 ng/mL for Cu(II), 0.16 ng/mL for Pd(II), and 0.8 ng/mL for Ag(I). The applicability and the accuracy of the developed method were estimated by the analysis of Ni(II) in hydrogenated oil (ghee) samples and Pd(II) in palladium charcoal.


2019 ◽  
Vol 57 (3) ◽  
pp. 336
Author(s):  
Luong Thi My Hanh ◽  
Nguyen Thi Minh Diep ◽  
Pham Thi Ngoc Mai ◽  
Nguyen Xuan Truong

A simple reversed phase HPLC method with UV detection has been successfully developed and validated for determination of moxifloxacin in human plasma. The sample pretreatment involves only single-step protein precipitation with tricloroacetic acid. Moxifloxacin was measured in plasma using a validated HPLC method with UV detector at 295 nm, C18 column (25cm×4.5mm, 5µm), a mixture of phosphate buffer pH 4.0 and acetonitrile (70:30, v/v) as mobile phase at a flow rate of 0.8 ml/min. Retention time of moxifloxacin was found to be 7.4 min. The mean recovery for the drug was obtained 97.30%. The calibration curve was linear over the concentration range of 0.3 to 25.0 µg/mL with coefficient correlation of 0.9991. This method was successfully applied for therapeutic drug monitoring.


2017 ◽  
Vol 17 (1) ◽  
pp. 54
Author(s):  
Dion Notario ◽  
Sudibyo Martono ◽  
Zullies Ikawati ◽  
Arief Rahman Hakim ◽  
Fathul Jannah ◽  
...  

A simple and rapid high-performance liquid chromatography method was developed and validated for quantifying LEV in human plasma. Chromatographic separation was performed under isocratic elution on a Luna Phenomenex® C18 (150 × 4.6 mm, 5 µm) column. The mobile phase was comprised of acetonitrile, methanol, and phosphate buffer 25 mM pH 3.0 (13:7:80 v/v/v) and pumped at a flow rate of 1.5 mL/min. Detection was performed by UV detector at a wavelength of 280 nm. Samples were pre-treated with acetonitrile followed by centrifugation, evaporation, and reconstitution step. The method proved linear (r = 0.995), sensitive (LLOQ and LOD was 1.8 and 0.6 µg/mL respectively), accurate (% error above LLOQ ≤ 12% and LLOQ ≤ 20%), precise (RSD ≤ 9%), robust in the ranges of 1.8-28.8 µg/mL, rapid (separation time not more than 10 min), and simple (use no organic additive in mobile phase). The method was showed reliable for quantifying LEV in human plasma.


2005 ◽  
Vol 19 (10) ◽  
pp. 783-787 ◽  
Author(s):  
Sung-Hee Cho ◽  
Ho-Taek Im ◽  
Wan-Su Park ◽  
Yong-Hwa Ha ◽  
Young-Wook Choi ◽  
...  

2004 ◽  
Vol 72 (2) ◽  
pp. 143-155 ◽  
Author(s):  
M. Sultan ◽  
H. Abdine ◽  
N. Zoman ◽  
F. Belal

A reversed-phase HPLC method with spectrophotometric detection was developed for the simultaneous determination of labetalol (LBT) and hydrochloro-thiazide (HCD). The chromatographic separation was performed using a Microbondapak C18 column (4.6 i.d. x 250 nm) and paracetamol as internal standard. A mobile phase consisting of 0.05 M phosphate buffer/acetonitrile of pH 4 (7:3) at a flow rate of 0.7 ml/min was used. The detection was affected spectrophotornetrically at 302 nm. The working concentration range was 0.3–10 µg/ml with detection limits of 0.05 µg/ml for both drugs. The lower quantitation limit was 0.25 µg/ml in the two cases. The method was successfully applied to tablets, the % recoveries were 99.45 ± 0.68 for LBT and 99.79 ± 0.75 for HCD. The method was extended to the in-vitro determination in spiked human plasma. The % recoveries were 91.12 ± 0.33 for LBT and 91.37 ± 0.40 for HCD. The interday and intraday precision and accuracy were evaluated in plasma by calculating the % RSD (n=5) and the % error and were found to be in the ranges of 1.18–4.1% and 0.38–0.36% for both drugs, respectively.


Author(s):  
Raju Chandra ◽  
Manisha Pant ◽  
Harchan Singh ◽  
Deepak Kumar ◽  
Ashwani Sanghi

A reliable and reproducible reversed-phase high performance liquid chromatography (RP-HPLC) was developed for the quantitative determination of Remipril drug content from marketed bulk tablets. The active ingredient of Remipril separation achieved with C18 column using the methanol water mobile phase in the ratio of 40:60 (v/v). The active ingredient of the drug content quantify with UV detector at 215 nm. The retention time of Remipril is 5.63 min. A good linearity relation (R2=0.999) was obtained between drug concentration and average peak areas. The limit of detection and limit of quantification of the instrument were calculated 0.03 and 0.09 µg/mL, respectively. The accuracy of the method validation was determined 102.72% by recoveries method.


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