scholarly journals Measurement of HDO Products Using GC-TCD: Towards Obtaining Reliable Analytical Data

2018 ◽  
Vol 5 (1) ◽  
pp. 1-11 ◽  
Author(s):  
Oman Zuas ◽  
Harry Budiman ◽  
Dieni Mansur ◽  
Muhammad Rizky Mulyana
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Analytical Data ◽  
Sample Treatment ◽  
Gaseous Products ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Method Development And Validation ◽  
Development And Validation

Abstract This paper reported the method development and validation of a gas chromatography with thermal conductivity detector (GC-TCD) method for the measurement of the gaseous products of hydrodeoxygenation (HDO). The method validation parameters include selectivity, precision (repeatability and reproducibility), accuracy, linearity, limit of detection (LoD), limit of quantitation (LoQ), and robustness. The results showed that the developed method was able to separate the target components (H2, CO2, CH4 and CO) from their mixtures without any special sample treatment. The validated method was selective, precise, accurate, and robust. Application of the developed and validated GC-TCD method to the measurement of by-product components of HDO of bio-oil revealed a good performance with relative standard deviation (RSD) less than 1.0% for all target components, implying that the process of method development and validation provides a trustworthy way of obtaining reliable analytical data.

scholarly journals THE RAPID AND GREEN HAIR ANALYSIS METHOD DEVELOPMENT USING FTIR FOR PAPAVERINE HCL DETERMINATION

2019 ◽  
pp. 211-217 ◽  
Author(s):  
ILMA NUGRAHANI ◽  
STEPHANIE SULISTIANA ◽  
SLAMET IBRAHIM
Keyword(s):  
Hair Sample ◽  
Method Development ◽  
Limit Of Detection ◽  
Area Under The Curve ◽  
Forensic Analysis ◽  
Percent Recovery ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Papaverine Hydrochloride

Objective: This study was aimed to develop a rapid analysis using FTIR (Fourier Transform Infra-Red) for papaverine hydrochloride (HCl) determination in the hair sample, supported by a mathematically manipulation; which never been reported before in toxicology and forensic analysis. Methods: Firstly, the method was checked its validity to ensure the feasibility for the quantitative purpose. The absorbance spectrums were collected by measure the drug, matrix, and its mixture. A spectra which showed the best specificity and linearity then was selected and derived. Afterwards, the area under the curve (AUC) was measured. A series of concentration was used for compose the calibration curve. Based on the result, some validation parameters were checked thoroughly. Further, for sample preparation, hair was collected non-invasively, then was decontaminated using soap. Next, it was immersed into a papaverine HCl solution at a concentration of 25 mg/ml along days. Finally, the amount of drugs absorbed were measured by the developed method using FTIR. Results: Experimental data showed that all validation parameters could be fulfilled by the developed method. The selected spectra for the content determination was 1320-1230 cm-1. Its linearity was represented by a correlation coefficient value (r) ≥ 0.9999, variation coefficient (Vxo) ≤ 2.0%. The limit of detection (LOD) was 0.00618% w/w, meanwhile, the limit of quantitation (LOQ) was 0.02060% w/w, respectively. The percent recovery was in the range 97-103% with the relative standard deviation (RSD) was ≤ 2.0%. The drug has detected after 72 h immersion, moreover, after 192 h the concentration gained was 0.1594±0.0011% w/w. Conclusion: As the conclusion, FTIR absorbance-derivative method is adequate as a rapid procedure for determine papaverine HCl in the hair sample. This method shows the appropriate of specificity, accuracy and precise. In addition, it shows the advantages of simplicity, green/eco-friendlier, and cost-efficiency.

scholarly journals ULTRAVIOLET-SPECTROPHOTOMETRIC METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF NORFLOXACIN PRESENT IN TASTE MASKED DRUG RESIN COMPLEX

2018 ◽  
Vol 11 (4) ◽  
pp. 244
Author(s):  
Ayya Rajendra Prasad ◽  
Jayanthi Vijaya Ratna
Keyword(s):  
Spectrophotometric Method ◽  
Absorption Maximum ◽  
Method Development ◽  
Limit Of Detection ◽  
Statistical Parameters ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Validation Parameters ◽  
Development And Validation

 Objective: The objective of this study was developed and validated a novel, specific, precise, and simple ultraviolet (UV)-spectrophotometric method for the estimation of norfloxacin present in taste masked drug-resin complex.Methods: UV-spectrophotometric determination was performed with ELICO SL 1500 UV-visible spectrophotometer using 0.1 N HCl as a medium. The spectrum of the standard solution was run from 200 to 400 nm range for the determination of absorption maximum (λ max). λ max of norfloxacin was found at 278 nm. The absorbance of standard solutions of 1, 2, 3, 4, and 5 μg/ml of drug solution was measured at an absorption maximum at 278 nm against the blank. Then, a graph was plotted by taking concentration on X-axis and absorbance on Y-axis which gave a straight line. Validation parameters such as linearity and range, selectivity and specificity, limit of detection (LOD) and limit of quantification (LOQ), accuracy, precision, and robustness were evaluated as per the International Conference on Harmonization (ICH) guidelines.Results: Linearity for the UV-spectrophotometric method was noted over a concentration range of 1–5 μg/ml with a correlation coefficient of 0.9995. The LOD and LOQ for norfloxacin were found at 0.39 μg/ml and 1.19 μg/ml, respectively. Accuracy was in between 99.00% and 99.17%. % relative standard deviation for repeatability, intraday precision, and interday precision was found to be 0.600, in between 0.291 and 0.410, and in between 0.682 and 1.439, respectively. The proposed UV spectrophotometric method is found to be robust.Conclusion: The proposed UV-spectrophotometric method was validated according to the ICH guidelines, and results and statistical parameters demonstrated that the developed method is sensitive, precise, reliable, and simple for the estimation of norfloxacin present in taste masked drug-resin complex.

Key Aspects of Analytical Method Development and Validation

2019 ◽  
Vol 31 (1) ◽  
pp. 32-39
Author(s):  
Suman Shrivastava ◽  
Pooja Deshpande ◽  
S. J. Daharwal
Keyword(s):  
Method Validation ◽  
Analytical Method ◽  
Method Development ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Method Development And Validation ◽  
Key Aspects ◽  
Development And Validation

Development of a method is crucial for discovery, development, and analysis of medicines in the pharmaceutical formulation. Method validation could also be thought to be one in all the foremost well-known areas in analytical chemistry as is reproduced within the substantial variety of articles submitted and presented in peer review journals every year. Validation of an analytical procedure is to demonstrate that it's appropriate for its intended purpose. Results from method validation are often wont to decide the quality, reliability and consistency of analytical results. Analytical methods need to be validated or revalidated. This review describes general approach towards validation process and validation parameters to be considered during validation of an analytical method. It also refers to various regulatory requirements like WHO, USFDA, EMEA, ICH, ISO/IEC. The parameters described here are according to ICH guidelines which include accuracy, precision, specificity, limit of detection, limit of quantification, linearity range and robustness.

Formulation, method development and validation of water soluble vitamins B1, B2 & B6 in bulk and tablet dosage form by HPTLC method

2018 ◽  
Vol 5 (1) ◽  
pp. 1-4
Author(s):  
Devi Velmurugan ◽  
Jambulingam Munusamy ◽  
Ananda Thangadurai Subramaniam ◽  
Anandkumar Karunakaran ◽  
Abdul Latiff MKM ◽  
...  
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Water Soluble ◽  
Good Resolution ◽  
Limit Of Quantitation ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Tablet Dosage ◽  
Hptlc Method

In the present study we are reporting  dissolution, method development and validation of water soluble vitamins B1, B2 & B6 in bulk and tablet dosage form by HPTLC method. The method is based on separation of the three vitamins using HPTLC. Thin layer chromatographic plates coated with silica gel 60F254 as the stationary phase and acetonitrile:water (6:4 v/v) as mobile phase. The chromatographic analysis was carried out in the reflectance and absorbance mode at 280 nm. The method was validated with respect to linearity, accuracy and precision, limit of detection and limit of quantitation. It was then applied for analysis of vitamins B1, B2 & B6 in combined tablet dosage form. The above method developed was reproducible with good resolution and the results of analysis have been validated with correlation coefficient of 0.9990

scholarly journals Method Development and Validation for Determination of Voglibose in Tablet Formulation Using LC-MS/MS

2011 ◽  
Vol 8 (4) ◽  
pp. 1770-1783
Author(s):  
Mithlesh Rajput ◽  
Meenakshi Dahiya ◽  
Premlata Kumari ◽  
Kamini Kalra ◽  
Manjeet Aggarwal ◽  
...  
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Limit Of Quantitation ◽  
Positive Mode ◽  
Method Development And Validation ◽  
Treatment Of Diabetes ◽  
Tablet Formulations ◽  
Development And Validation

Voglibose is a potent α glucosidase inhibitor, used for the treatment of diabetes mellitus. For quantitative determination of voglibose in pharmaceutical formulations of low doses, simple, sensitive, accurate and precise LC-MS/MS method using electrospray ionization in positive mode was developed and validated. The method was found linear in the concentration range of 25.0-1200 ηg/mL with a correlation coefficient of 0.9998. The limit of detection (LOD) of the method was found to be 1.5 ηg/mL and limit of quantitation (LOQ) was achieved at 3.0 ηg/mL. The recoveries of voglibose from spiked samples at different concentration levels were found in the range of 98-102%. The proposed method was found suitable for quantitation of voglibose and for the determination of uniformity of content of the dosage units of the tablet formulations.

scholarly journals HPLC METHOD DEVELOPMENT AND VALIDATION FOR AZITHRO-MYCIN IN ORAL SUSPENSION

2019 ◽  
pp. 7-12
Author(s):  
Alok Pratap Singh ◽  
Iti Chauhan ◽  
Snigdha Bhardwaj ◽  
Praveen Gaur ◽  
S Sadish Kumar ◽  
...  
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Validation Parameters ◽  
Wide Range ◽  
Tract Infections ◽  
Development And Validation

Introduction: Azithro-mycin a semi-synthetic, azalide congener of erythro-mycin indicated in the treatment of respiratory tract infections. Various methods available for determination of Azithro-mycin, but HPLC are most versatile one. Objective: The present study is based on the development and validation of a rapid, simple high performance liquid chromatography (HPLC) method equipped with UV detector for quantitative analysis of Azithro-mycin (AZN) in suspension. Material and methods: The Method was performed by using Hypersil BDS-C18 (250 mm × 4.6 mm i.d.) column MS-II, with an isocratic mobile phase of methanol, acetonitrile and phosphate buffer pH 8 (60:30:10; v/v) with run time 15 minutes. The determinations were performed at a flow rate of 1.0ml/min, and UV detector set at 212 nm. Result and Discussion: The method was found to be specific with relative standard deviation (RSD) less than 2.09%. The method showed accuracy with RSD less than 1.34% and precision in repeatability with RSD less than 1.42%. The method was found to be linear over a wide range of concentration from 1.0 to 50.0 μg/mL (R2 = .995). Limit of detection and limit of quantification were found to be 14.40 ng/mL and 43.66 ng/mL respectively. Conclusion: It was advantageous to use UV detector over other methods employing electrochemical, photodiode array etc. as the detector, because of cheap and easy availability. The developed method fulfilled all validation parameters as per ICH and can be successfully applied to quantify percent drug content in marketed oral Azithro-mycin suspension.

scholarly journals Analytical method development and validation studies for the estimation of H2 receptor antagonist drug (Ranitidine)

2021 ◽  
Vol 7 (2) ◽  
pp. 85
Author(s):  
Renuka Manjunath ◽  
Deepak Kumar Jha
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Pharmaceutical Preparation ◽  
H2 Receptor Antagonist ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation

<p class="abstract"><strong>Background:</strong> An analytical science in the development, finding a new molecules and procreation of pharmaceuticals has been an extensive approached. From the evaluation over small quantities of complex biological substances to the quality monitoring of the finished dosage form, the use on analytical technology know- how covers an ample thoroughness over techniques or disciplines.</p><p class="abstract"><strong>Methods:</strong> Reversed phase high performance liquid chromatography (RP-HPLC) approach has been promoted for the discernment over Ranitidine (RAN) within pharmaceutical dosage form split of RAN was accomplished inside a unaccompanied chromatographic run of an Phenomenix column size 5 μm 4.6x250 mm along with UV analysis at 227 nm wavelength, below isocratic conditions, using Ammonium acetate and Methanol (pH 6.0) in 80:20 ratio. Validation parameters had been observed in accordance with exhibit linearity, accuracy, precision, Limit of Quantitation and Limit of detection in conformity in imitation of ICH guidelines.  </p><p class="abstract"><strong>Results:</strong> The contemporary approached demonstrates significant linearity upon the range concerning 50-202.5 μg/ml for RAN followed by intra-day and inter-day precision, expressed so the relative standard deviation (RSD), on replicates is &lt;2.0 and accuracy among the range over 98-102%.</p><p class="abstract"><strong>Conclusions:</strong> The flourished RP-HPLC technique was once innovative, suitable for detecting RAN in pure form and in pharmaceutical preparation.</p>

scholarly journals Development and Validation of Estimation of Genotoxic Impurity (Triethyl orthoformate content) in 5-methyl-4-isoxazole carboxylic acid (5-MIA) by using GC Technique

2021 ◽  
Vol 37 (2) ◽  
pp. 348-353
Author(s):  
Mohan bhatale ◽  
Neelakandan kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Gurunathan ramalingam
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Fused Silica ◽  
Triethyl Orthoformate ◽  
Concentration Limit ◽  
Simultaneous Estimation ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Gas Chromatographic Method ◽  
Development And Validation

A simple, selective, precise and accurate Gas chromatographic method for determination of Triethyl orthoformate content (Genotoxic impurity) in 5-MIA is reported. The GC method development and validation as per the International Council for Harmonisation (ICH) guidelines Q2(R1). The effective chromatographic separations were achieved on DB-624, 60 m × 0.53 mm ID, with film thickness of 3.0 μm (Fused silica capillary column), Capillary injector temperature of 150°C, and Nitrogen Carrier gas. This method is unique as there is no UV response; hence GC Method was developed for Triethyl orthoformate. The elution was accomplished with the flow rate of 5.0 mL/min and Split Flow of 10 mL/minute. Detection was performed with FID detector (temp. 260°C) and with column oven temperature program. Methods range from limit of quantitation (LOQ) to 150% level with respect to specification concentration limit of impurity is linear and correlation coefficient of impurity is > 0.99. The linearity of Triethyl orthoformate covered from LOQ to 113 ppm (ie. LOQ to 150% of specification limit) and LOQ to 19 ppm wrt standard concentration. The limit of detection (LOD)values were observed were 2.5 ppm and limit of quantitation (LOQ) were 7.7 ppm, respectively. The parameters selected for the method validated were from international conference on harmonization guidelines, Indian pharmacopeia, USP. The percentage recovery from LOQ, 50% ,100% to 150% level of content were 87.70%, 98.60%, 102.25 and 96.59% respectively. The %RSD values were for LOQ to 150% were from 1.64%, 0.89%, 1.78 % and 1.49%. The range was covered from LOQ to 150% of standard concentration. The results of validation parameters were found in the acceptance range. Standard and sample were stable up to 30 h at when stored at room temperature. Also it was quite robust for the small change in method parameter like, change in column oven temperature(± 5 degree). Hence from the above parameter it was concluded that the GC method with FID detector is selective, precise, linear, and robust for simultaneous estimation of Triethyl orthoformate in Drug Substances.

scholarly journals ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR STABILITY INDICATING HPTLC METHOD FOR ASSAY OF STIRIPENTOL IN BULK AND DOSAGE FORM

2021 ◽  
Vol 3 (4) ◽  
pp. 26-30
Author(s):  
Santosh Kumar Kashid ◽  
Amit Tapkir ◽  
Pravin Choudhari
Keyword(s):  
Room Temperature ◽  
Method Development ◽  
Limit Of Detection ◽  
Acidic Condition ◽  
Calibration Plot ◽  
Stability Indicating ◽  
Study Results ◽  
Limit Of Quantitation ◽  
Method Development And Validation ◽  
Development And Validation

Introduction: This work is concerned with the stability-indicating method development and validation of Stiripentol in a bulk drug and formulation by high-performance thin-layer chromatographic method (HPTLC). Materials and Methods:The pre-coated silica gel 60 F254 aluminum plate was selected as the stationary phase, and the solvent system consisted of Ethyl acetate: Dichloromethane: Toluene (2:2:6 v/v) used as developing solvents. Analysis of Stiripentol was carried out at 301 nm with Stiripentol being detected at an R(f) of 0.63. The developed method was validated for linearity, accuracy, precision, limit of detection (LoD), limit of quantitation (LoQ), robustness parameters, and stability are determined by force degradation study. Results and Discussion: The correlation coefficient of Stiripentol was 0.994 observed. The calibration plot was linear between 50–300 ng/band, respectively. The average percentage recovery of Stiripentol was found to be 100.25 %. Intra and inter-day precision measured as %RSD was less than 2%. Hence stability study of Stiripentol, it was found to degrade in acidic condition(8.52% - 0.1N HCL for 30 minutes at room temperature), alkali condition(7.47%- 0.1 N NaOH for 30min at room temperature), Hydrolytic condition(4.73%– dist. Water for 30min at room temperature), thermal condition(7.69%-40°C for 30min ), oxidative condition(7.55% - 3% H2O2 for 30min at room temperature) and photolytic UV condition(7.54% -24hr UV radiation) respectively. Stiripentol was unstable in acidic condition and stable in normal dist. Water hydrolytic condition. Conclusion: The proposed method was found to be very sensitive and accurate for the determination of Stiripentol in bulk and formulation.

scholarly journals UV Spectrophotometric Method Development and Validation of Esomeprazole in Bulk and Pharmaceutical Dosage Forms

2021 ◽  
Vol 12 (3) ◽  
pp. 2286-2290
Author(s):  
Gowtham Reddy Cheruku ◽  
Sai Laasya Mithinti ◽  
Purushotham Saidu
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Regression Equations ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Technical Requirements ◽  
Relative Standard ◽  
Method Development And Validation ◽  
Development And Validation

The work discusses method development and validation. An uncomplicated, accurate, and straightforward method was developed for the drug Esomeprazole in bulk as well as Pharmaceutical dosage form. NaOH was used as the solvent. The maximum wavelength (ʎ max) for Esomeprazole was found to be 305nm. The validation was performed as per International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH) guidelines for Accuracy linearity, precision, Limit of Detection (LOD) and Limit of Quantification (LOQ). Esomeprazole's recovery percentage (%) was 100.20%, respectively. Linearity for Esomeprazole was observed between 5-25µg/ml, respectively. Regression equation y=0.0407x-0.0122, regression coefficient (r²) is 0.9963 for Esomeprazole. Inter day and intraday precision were checked, % relative standard deviation values were less than 2. The regression equations were used to derive the Limit of Detection (LOD) and Limit of Quantification (LOQ) values. LOD value was found to be 0.734 µg/mL and LOQ value was 2.224 µg/mL for Esomeprazole. The assay of the marketed formulation was performed, which was between 98-102%.  So the method developed was simple and economical that can be adopted for routine tests. 

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