scholarly journals PENETAPAN KADAR METANOL HASIL DESTILASI PENGUAP VAKUM PUTAR EKSTRAK METANOL DAUN UBI UNGU MENGGUNAKAN RAMAN SPEKTROFOTOMETER

2018 ◽  
pp. 13
Author(s):  
Santi Maha Dewi
Keyword(s):  
Limit Of Detection ◽  
Pressure Variation ◽  
Vacuum Pressure ◽  
Assay Method ◽  
Absolute Methanol ◽  
Limit Of Quantification ◽  
Purple Sweet Potato ◽  
Non Destructive ◽  
Curve Equation ◽  
Rotary Vacuum

Solvent extracted results are often not utilized for re-extraction. Methanol is a universal solvent which is often used as an extract of simplicia. The result of a rotary vacuum evaporator distillation is not known purity and level. Raman spectrosphotometer is a non destructive method of analysis that can be applied to determine the levels and purity of distilled methanol. The objective of this research is to know the change of vacuum pressure to the level and purity of methanol, so that methanol from rotary vacuum distillation can be reused for re-extraction. Purple sweet potato leaves are macerated using 95% methanol : 3% citric acid. The extract was evaporated using a rotary vacuum evaporator at 100 mbar, 150 mbar, and 200 mbar vacuum pressure with a range of 5 to 180 min. Purity and methanol levels were determined using a Raman Handheld 1064 nm spectrophotometer. Validation of methanol assay method with Raman spectrophotometer was obtained: precision: KV 0.19% -1.70%, accuracy: 94.4-103.8%, limit of detection: 1.77% (v/v), limit of quantification: 5.89% (v/v), the range of linearity of 1.77% -99.9% (v/v), with a calibration curve equation: y = 216,88x + 1437.1 and the value of R2 = 0.9997. Methanol content of distillation product with pressure variation 100 - 200 mbar in the span of 5 to 180 minutes obtained methanol level 59.8-81.2% (v/v). All distilled methanol yields a spectrum similarity of 86-99% when compared with absolute methanol.

scholarly journals UPLC Method Optimisation and Validation for the Estimation of Sodium Cromoglycate in Pressurized Metered Dosage Form

2017 ◽  
Vol 2 (02) ◽  
pp. 18-24
Author(s):  
Anas Rasheed ◽  
Osman Ahmed
Keyword(s):  
Sodium Cromoglycate ◽  
Orthophosphoric Acid ◽  
Limit Of Detection ◽  
Calibration Graph ◽  
Assay Method ◽  
Dose Inhaler ◽  
Limit Of Quantification ◽  
Adequate Accuracy ◽  
Metered Dose ◽  
Ich Guideline

UPLC assay method optimised and validated for sodium cromoglycate in metered dose inhaler (MDI) using metronidazoleas an internal standard.The separation of Sodium Cromoglycate was achieved on Hypersil BDS C18 (100 mm x 2.1 mm, 1.7 μm) with gradient mobile phase containing methanol, orthophosphoric acid and acetonitrile in the ratio of 50:15:35 %v/v/v. The flow rate was 0.25 mLmin-1, injection volume 20μl and detection wavelength was set at 326nm, at ambient temperature. The validation of the proposed method was carried outfor linearity, accuracy, precision, robustness, limit of detection and limit of quantification test as per ICH guideline. The retention time of sodium cromoglycate found to be 4.73 min. Calibration graph was found to be linear at range 8- 40μg/ml. The regression coefficient (r2) was found tobe 0.9978.The proposed method was rapid with adequate accuracy, precision, ruggedness and robustness and hence be suitable for theroutine analysis of sodium cromoglycate in meter dose inhalation and in bulk.

scholarly journals NON-DESTRUCTIVE RAMAN SPECTROSCOPIC METHOD FOR ESTIMATION OF MONTELUKAST FROM TABLET DOSAGES FORM

2017 ◽  
Vol 9 (6) ◽  
pp. 161
Author(s):  
Jwal Doctor ◽  
Palak Thakkar ◽  
Mitul Prajapati ◽  
Nrupresh Patel ◽  
Priti J. Mehta
Keyword(s):  
Limit Of Detection ◽  
Process Analysis ◽  
Spectroscopic Method ◽  
Pharmaceutical Products ◽  
Integration Time ◽  
Limit Of Quantification ◽  
Raman Spectroscopic ◽  
Quality Checks ◽  
Technology Tool ◽  
Non Destructive

Objective: A rapid, non-destructive and non-solvent raman spectroscopic method for estimation of Montelukast from tablet dosages form Methods: Quantification was carried out by measuring the intensity of analyte peak at 1440 cm-1. Each Raman spectrum corresponded to an accumulation of 4 scans with an exposure time of 5 sec for each scan with a total integration time of 20 sec.Results: The method exhibited linearity between 2 mg-24 mg show well resolve quantification From MON. The linearity equation was calculated as y = 13.036x+70.819 and the correlation coefficient was found to be 0.997 for MON. LOD (limit of detection) and LOQ(limit of quantification) values were calculated using the calibration curve slope and standard deviation of the response. The LOD (limit of detection) and LOQ (limit of quantification) values were found to be 1.71 mg and 5.13 mg respectively.Conclusion: The developed method was successfully applied for assay of montelukast in the intact formulation. The method was validated according to an international conference on harmonisation guidelines. A recent study, montelukast sodium had been analysed by the raman method, but, looking into the tremendous potential of raman spectroscopic method; it can be extended as a process analysis and technology tool in various quality checks during manufacturing of pharmaceutical products.

scholarly journals A Validated RP-HPLC Method for Estimation of Related Compounds in Hydroxy Naproxen

2020 ◽  
Vol 32 (5) ◽  
pp. 1158-1164
Author(s):  
L. Vaikunta Rao ◽  
K. Tirumala Rao ◽  
V.V. Krishna Mohan Kandepi
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Assay Method ◽  
Array Detector ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Related Substance ◽  
Mobile Phase Flow Rate ◽  
Rp Hplc ◽  
Related Compounds

A simple, linear gradient liquid chromatographic method (RP-HPLC) is proposed for the simultaneous estimation of related compounds in hydroxy naproxen samples. Chromatographic separation was achieved on Zorbax SB C8 (150 × 4.6) mm, 3.5 μm particle size RRLC short column and eluent A used as 0.1% v/v trifluoroacetic acid in water and eluent B used as acetonitrile using Agilent RRLC (UHPLC) system. The mobile phase flow rate was 1.0 mL/min and the eluted compounds were monitored at 235 nm for related substance method and assay method. The excellent resolution was obtained between hydroxy naproxen and its related compounds, which were eluted within 25 min. The performance of the method was validated with respect to ICH guidelines for specificity, limit of detection, limit of quantification, linearity, accuracy, precision and robustness. The correlation coefficient(r) was > 0.995 for both the methods from linearity data and percentage of recovery is 98.0 to 102.0 for assay method and 80.0 to 120.0% for related substance method. Sensitivity of the method was found be less than 0.5 μg/mL. Peak homogeneity data for naproxen in the chromatograms from the selectivity solution obtained by use of the photodiode array detector demonstrated the specificity of the method for analysis of hydroxy naproxen in presence of the related compounds

scholarly journals A Stability Indicating Assay Method Development and Validation for the Frovatriptan Succinate Monohydrate by Using UV: A Spectrophotometric Technique

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Hitesh Verma ◽  
Surajpal Verma ◽  
Harmanpreet Singh
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Assay Method ◽  
Forced Degradation ◽  
Solution Stability ◽  
Limit Of Quantification ◽  
Experimental Conditions ◽  
Stability Indicating ◽  
Ich Guidelines ◽  
Relative Standard

A new simple, reliable, inexpensive, and accurate method was developed for the quantification of Frovatriptan Succinate Monohydrate in different physiological media at 244 nm in bulk and in tablet dosage forms. The developed method is an attempt to surpass the disadvantages associated with the reported methods, namely, less sensitive and tedious in usage for routine purposes. Beer’s law was followed over the range of 1.0 µg/mL to 4.5 µg/mL. Stability indicating assay method was developed and validated as per the ICH guidelines using various parameters, for example, accuracy, precision, limit of quantification, limit of detection, robustness, ruggedness, solution stability, recovery, forced degradation (hydrolysis, photo degradation, thermal degradation, and oxidation), and so forth. Percent relative standard deviation associated with all the parameters was less than 2, showing compliance with the acceptance criteria of ICH guidelines. The developed method was very sensitive as limit of quantification and limit of detection were found to be 0.025 µg/mL and 0.00625 µg/mL, respectively. Forced degradation studies of drug reveal good stability under the chosen experimental conditions.

scholarly journals CONTENT VARIATIONS OF CARBAMAZEPINE TABLETS IN IRAQI COMMUNITY PHARMACIES: APPLICATION OF HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY ASSAY METHOD

2018 ◽  
Vol 11 (2) ◽  
pp. 117
Author(s):  
Mohanad Naji Sahib
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
High Standard ◽  
Assay Method ◽  
Solution Stability ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Middle East Countries

 Objective: There is paucity in the literature and documentation regarding the post-marketing product quality in Iraq and Middle East countries in general. Therefore, a simple reverse phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the determination of carbamazepine (CMZ) content in post-marketed tablet dosage form.Methods: The RP-HPLC analysis was run at a flow rate of 1 ml/min with a mixture of methanol: water (70:30) mobile phase using a Thermo Synchronise C18 column at a UV detection wavelength of 230 nm. The method was validated for selectivity, linearity, precision, accuracy, limit of detection (LOD), limit of quantification (LOQ), solution stability, and robustness.Results: The calibration curve was linear over a concentration range of 1–20 μg/ml (r2=0.9999) with LOD and LOQ of 0.01 and 0.04 μg/ml, respectively. The intraday and interday precision and accuracy were between 0.04–1.67% and 0.04–0.78%, respectively. The results of analysis of the four brands of CMZ tablets were passed the European Pharmacopoeia specification but with a high standard deviation of mean drug content of some brands.Conclusion: This study shows that the quality of post-marketed drugs and/or the storage conditions in developing countries must be carefully assessed for a better therapeutic response.

Chromatographic Quantification of Ivermectin and Pranziquantel in the Tablets Using Stability Indicating RP-HPLC Method

2019 ◽  
Vol 25 (3) ◽  
pp. 254-261
Author(s):  
Naga Venkata Suresh Kumar Devaka ◽  
Vallabhaneni Madhusudhan Rao
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Assay Method ◽  
Array Detector ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Relative Standard

Background: A new stability indicating RP-HPLC based assay method was developed to quantify ivermectin and praziquantel simultaneously and applied effectively to tablets. Methods: The simultaneous assay of ivermectin and praziquantel by RP-HPLC was done using an YMC C18 (250 mm × 4.6 mm, 5 µm) column with a mobile phase mixture of 0.1M disodium hydrogen phosphate (pH 4.5) and acetonitrile (55:45, v/v) using a isocratic flow rate of 1.0 ml/min and measured at 242 nm using photodiode array detector. All parameters were validated following the ICH guiding principles. The method was applied to quantify ivermectin and praziquantel simultaneously in tablets. Results: The retention values of ivermectin and praziquantel were 3.465 min and 4.468 min, respectively. The method’s linearity was found to be 1-3 µg/ml (ivermectin) and 25-75 µg/ml (praziquantel). The limit of detection was 0.010 µg/ml (ivermectin) and 0.046 µg/ml (praziquantel); limit of quantification was 0.033 µg/ml (ivermectin) and 0.155 µg/ml (praziquantel). The percent relative standard deviation of ivermectin and praziquantel was ˂1.0%. The percent assay was 99.51% and 99.20% for ivermectin and praziquantel, respectively. In tablets, the percent recovery of ivermectin and praziquantel was 99.60% and 99.38% with a percent relative standard deviation value of 0.353% and 0.106%, respectively. Stability indicating capability of the method was demonstrated through the stress degradation studies. Conclusion: The developed method was proved to be selective, precise and accurate for the quality control of ivermectin and praziquantel in tablets.

Development and Validation of Stability Indicating Assay Method for Simultaneous Estimation of Glibenclamide and Metformin

2017 ◽  
Vol 8 (03) ◽  
Author(s):  
Waje M. K. ◽  
Barge V. U. ◽  
Talole B. B.
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Assay Method ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Chromatographic Procedure ◽  
Development And Validation ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A high performance reverse phase liquid chromatographic procedure is developed for simultaneous estimation of Metformin and Glibenclamide in combined tablet dosage form. The method was carried out on Agilent Hypersil ODS (4.6 x 250 mm) column with a mobile phase used consisting of Methanol: Water (0.1 % OPA) OPA= Ortho Phosphoric acid (80:20) and the pH of buffer was adjusted to 3 using 2M Orthophosphoric acid. The detection of the combined dosage form was carried out at 228 nm and a flow rate employed was 1 ml/min and column oven temperature at 300C. The retention times of Metformin andGlibenclamide were 3.4667 and 7.3500 minutes respectively. The developed method was validated in terms of accuracy, precision, linearity, limit of detection, limit of quantification as per ICH norms. The proposed method can be used for the estimation of these combined drugs.

Spectrophotometeric Determination of Trifluoperazine HCL in Pure Forms and Pharmaceutical Preperations

2017 ◽  
Vol 9 (5) ◽  
Author(s):  
Mohammad Hamzah Hamzah ◽  
Rawa M M Taqi ◽  
Muna M. Hasan ◽  
Raid J. M. Al-Timimi
Keyword(s):  
Standard Method ◽  
Limit Of Detection ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Oxidizing Agent ◽  
Optimum Conditions ◽  
Limit Of Quantification ◽  
Cerium Ion ◽  
Blank Solution

A simple and accurate spectrophotometric method for the determination of Trifluoperazine HCl in pure and dosage forms was developed. The method is based on the reaction between Trifluoperazine HCl and p-chloroaniline in the presence of cerium ion as oxidizing agent which lead to the formation of violate color product that absorbed at a maximum wavelength 570nm while the blank solution was pink. Under the optimum conditions a linear relationship between the intensity and concentration of TRF in the range 4-50μg/ml was obtained . The molar absorptivity 3.74×103 L.mol-1.cm-1 , Limit of detection (2.21μg/ml), while limit of quantification was 7.39μg/ml. The proposed analytical method was compared with standard method using t-test and F-test , the obtained results shows there is no significant differences between proposed method and standard method. Based on that the proposed method can be used as an alternative method for the determination of TRF in pure and dosage forms.

Recent Trends in Development of Nanomaterials Based Green Analytical Methods for Environmental Remediation

2020 ◽  
Vol 16 ◽  
Author(s):  
Sidra Amin ◽  
Amber R. Solangi ◽  
Dilawar Hassan ◽  
Nadir Hussain ◽  
Jamil Ahmed ◽  
...  
Keyword(s):  
Optical Sensors ◽  
Environmental Remediation ◽  
Environmental Chemistry ◽  
Limit Of Detection ◽  
Environmental Pollutants ◽  
Toxic Metal ◽  
Electrochemical Analysis ◽  
Good Choice ◽  
Nano Materials ◽  
Limit Of Quantification

Background: In recent years, the occurrence and fate of environmental pollutants has been recognized as one of the emerging issues in environmental chemistry. A survey documented about a wide variety of these pollutants, which are often detected in our environment and these are major cause of shortened life spans and the global warming. These pollutants include toxic metal, pesticides, fertilizers, drugs and dyes released into soil and major water bodies. The presence of these contaminants causes major disturbance in eco-system’s balance. To tackle these issues many technological improvements are made to detect minute contaminations. The latest issue being answered by the scientists is the use of green nano materials as sensors which are economical, instant and give much better results at low concentrations and can be used for the field measurements resulting in no dangerous by-product that could lead to more environmental contamination. Nano materials are known for their wide band gap, enhanced physical and optical properties with option of tuneablity as per need, by optimizing certain parameters. They are proved to be good choice for analytical/optical sensors with high sensitivity. Objective: This review holds information about multiple methods that use green nanomaterials for the analytical assessment of environmental pollutants. UV-Vis spectrophotometry and electrochemical analysis using green and reproducible nanomaterials are the major focus of this review article. To date, there are number of spectrophotometric and electro chemical methods available that have been used for the detection of environmental pollutants such as toxic metals, pesticides and dyes. Conclusion: The use of nanomaterials can drastically change the detection limits due to having large surface area, strong catalytic properties, and tunable possibility. With the use of nano materials, lower than the marked limit of detection and limit of quantification were seen when compared with previously reported work. The used nano-materials could be washed, dried, and reused, which makes the methods more proficient, cost effective and environmentally friendly.

Calcium/Copper alginate framework doped with CuO nano-particles as a novel adsorbent for micro-extraction of benzodiazepines from human serum

2020 ◽  
Vol 16 ◽  
Author(s):  
Nadereh Rahbar ◽  
Fatemeh Ahmadi ◽  
Zahra Ramezani ◽  
Masoumeh Nourani
Keyword(s):  
Human Serum ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Nano Particles ◽  
Limit Of Quantification ◽  
Analytical Methodology ◽  
Fiber Fabrication ◽  
Relative Standard ◽  
Green Procedure

Background: Sample preparation is one of the most challenging phases in pharmaceutical analysis, especially in biological matrices, affecting the whole analytical methodology. Objective: In this study, a new Ca(II)/Cu(II)/alginate/CuO nanoparticles hydrogel fiber (CCACHF) was synthesized through a simple, green procedure and applied for fiber micro solid phase extraction (FMSPE) of diazepam (DIZ) and oxazepam (OXZ) as model drugs prior to high-performance liquid chromatography-UV detection (HPLC-UV). Methods: Composition and morphology of the prepared fiber were characterized and the effect of main parameters on the fiber fabrication and extraction efficiency have been studied and optimized. Results: In optimal conditions, calibration curves were linear ranging between 0.1–500 µg L−1 with regression coefficients of 0.9938 and 0.9968. Limit of detection (LOD) (S/N=3) and limit of quantification (LOQ) (S/N=10) of the technique for DIZ and OXZ were 0.03 to 0.1 µg L−1. Within-day and between-day relative standard deviations (RSDs) for DIZ and OXZ were 6.0–12.5% and 3.3–9.4%, respectively. Conclusion: The fabricated adsorbent has been substantially employed to extraction of selected benzo-diazepines (BZDs) from human serum real specimens and the obtained recoveries were also satisfactory (82.1-109.7%).

Sign in / Sign up

Export Citation Format

Share Document