scholarly journals A Validated TLC-Densitometric Method for the Determination of Mesterolone in Bulk Material and in Tablets

2015 ◽  
Vol 2015 ◽  
pp. 1-8 ◽  
Author(s):  
Małgorzata Dołowy ◽  
Alina Pyka-Pająk ◽  
Katarzyna Filip ◽  
Joanna Zagrodzka
Keyword(s):  
Limit Of Detection ◽  
Bulk Material ◽  
Phosphomolybdic Acid ◽  
Tablet Formulation ◽  
Phase System ◽  
Limit Of Quantification ◽  
Related Substance ◽  
Label Claim ◽  
Tlc Analysis

Mesterolone is a synthetic androgenic steroid indicating a weak anabolic activity. A new, simple in use, and economical TLC-densitometric method in normal phase system (NP-TLC) has been developed and validated for the identification and quantitative determination of mesterolone in bulk drug and in tablet formulation. NP-TLC analysis was performed on aluminium plates precoated with silica gel 60F254as the stationary phase using chloroform-acetone (40 : 10, v/v) as mobile phase. Densitometric analysis was carried out atλ=745 nm after staining with phosphomolybdic acid. These conditions were found to give visible (dark blue) spot and sharp peak, respectively, for mesterolone atRF  0.75±0.02and enabled satisfactory separation of mesterolone from its related substance (potential impurity). The proposed NP-TLC-densitometric method was validated for specificity, linearity, precision, accuracy, robustness, and sensitivity according to ICH guideline and other validation requirements. The limit of detection (LOD) and limit of quantification (LOQ) were 61.0 ng·spot−1and 184.0 ng·spot−1, respectively. The percent content of mesterolone in marketed tablet formulation was found to be 99.40% of label claim. The developed TLC-densitometric method can be successfully used in quality control of mesterolone in bulk material and also tablet formulation.

Development and Validation of a Quantitative NMR Method for the Determination of the Commercial Tablet Formulation of Sulfasalazine

2018 ◽  
Vol 15 (1) ◽  
pp. 39-44 ◽  
Author(s):  
Feng Su ◽  
Zi-qing Sun ◽  
Xian-rui Liang
Keyword(s):  
Maleic Acid ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Tablet Formulation ◽  
Quantitative Nmr ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Development And Validation ◽  
Good Agreement

Introduction: Quantitative NMR spectroscopy (qNMR) is a rapid, simple and efficient method for the assay of sulfasalazine (SSZ) in commercial tablet formulation. Materials and Methods: The qNMR method was demonstrated using maleic acid as an internal standard and DMSO-d6 as a solvent. The characteristic signals of SSZ at δ 8.36 ppm and maleic acid at δ 6.28 ppm were quantified. The reliability of the quantification method had been implemented successfully in validated experiments including specificity and selectivity, linearity, recovery, precision concentration rang, limit of detection (LOD), limit of quantification (LOQ), stability and robustness. Conclusion: The method was found to be liner (R2 = 0.9991) from 8.62 to 20.14 mg/0.6 mL DMSO-d6 in the drug concentration range. The maximum relative standard deviation (RSD) of recovery and precision were tested to be 0.59% and 0.65%, respectively. The LOD and LOQ were determined to be 0.02, 0.07 mg/mL, respectively. The RSD of stability was 0.05%. The robustness was demonstrated by changing four different parameters with the maximum difference less than 0.9%. In addition, the result of qNMR showed in good agreement with the HPLC and UV methods. Based on the experiments, the developed method was successfully applied to the determination of SSZ in commercial tablet.

scholarly journals Aqueous Two-Phase System–Ion Chromatography for Determination of Thiocyanate in Raw Milk

Separations ◽  
2021 ◽  
Vol 8 (11) ◽  
pp. 212
Author(s):  
Bin Jiang ◽  
Shaojing Zhong ◽  
Hongliang Yu ◽  
Peifeng Chen ◽  
Baoyun Li ◽  
...  
Keyword(s):  
Ion Chromatography ◽  
Limit Of Detection ◽  
Raw Milk ◽  
Enrichment Ratio ◽  
Phase System ◽  
Limit Of Quantification ◽  
Two Phase ◽  
Aqueous Two Phase System ◽  
Pre Treatment

Thiocyanate could effectively inhibit bacteria in milk and extend the shelf life of milk. However, excessive addition will lead to health risks. Therefore, the determination of thiocyanate in raw milk has received a lot of attention, but the determination could be interfered with by other components in raw milk and the pre-treatment of raw milk is complex. In this study, a new pretreatment method combined with ion chromatography (IC) for rapid and sensitive determination of thiocyanate is proposed. An acetonitrile/(NH4)2SO4 aqueous two-phase system (ATPS) was developed for the separation and enrichment of thiocyanate in raw milk. Response surface methodology was performed to optimize the extraction conditions and an efficient pretreatment were obtained using ATPS composed of 42% acetonitrile (w/w) and 16% (NH4)2SO4 (w/w), with the pH 4.7, and the recovery of thiocyanate reached 107.24 ± 0.5%, and the enrichment ratio was 10.74 ± 0.03. IC was used to establish a thiocyanate enrichment method. The linear range was from 0.05 to 15 mg/L and R2 = 0.998, the limit of detection (LOD) was 0.2 μg/L, the limit of quantification (LQD) was 0.6 μg/L. Hence, it is feasible to combine ATPS with IC for the enrichment and determination of thiocyanate in raw milk.

scholarly journals DEVELOPMENT AND VALIDATION OF HPLC-DAD METHOD FOR THE DETERMINATION OF BISOPROLOL IN TABLET DOSAGE FORMS

2017 ◽  
Vol 9 (6) ◽  
pp. 54 ◽  
Author(s):  
Yuliya Kondratova ◽  
Liliya Logoyda ◽  
Yuliia Voloshko ◽  
Ahmed Abdel Megied ◽  
Dmytro Korobko ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Label Claim ◽  
Development And Validation ◽  
Tablet Dosage

Objective: A rapid, simple and sensitive RP-HPLC method was developed and validated for the determination of bisoprolol fumarate in bulk and pharmaceutical dosage form.Methods: Chromatographic separation was achieved within 2.5 min on ACQUITY Arc System, Waters Symmetry C18 column (3.9 mm i.d. X 150 mm, 5 μm particle sizes) using a mobile phase consisted of acetonitrile: phosphate buffer (25:75 v/v) in an isocratic mode at a flow rate of 1.4 ml/min. The pH of the mobile phase was adjusted to 7.0 with orthophosphoric acid and UV detection was set at 226 nm.Results: The retention time for bisoprolol fumarate was found to be 2.09 min. The proposed method was validated according to ICH guidelines with respect to linearity, specificity precision, accuracy and robustness. The limit of detection and limit of quantification are calculated and found to be 0.4825 and 1.4621 μg/ml; respectively.Conclusion: The proposed method can help research studies, quality control and routine analysis with lesser resources available. The results of the assay of pharmaceutical formulation of the developed method are highly reliable and reproducible and is in good agreement with the label claim of the medicines.Keywords: Bisoprolol, High-Performance Liquid Chromatography, Validation, ICH guidelines

scholarly journals Development and validation of TLC densitometry method for the determination of Gliclazide in tablet dosage form

2012 ◽  
Vol 1 (10) ◽  
pp. 332-335
Author(s):  
Yuni Retnaningtyas ◽  
Lestyo Wulandari ◽  
Feby Erliana
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Regression Function ◽  
Pharmaceutical Journal ◽  
Limit Of Quantification ◽  
Label Claim ◽  
The Mean ◽  
Development And Validation ◽  
Tablet Dosage

Some tablet pharmaceutical preparations containing Gliclazide as sole active ingredient, are marked now in Indone-sia. The determination of the component of preparation both qualitatively and quantitatively is important to ensure quality of the product. This research is aimed to develop a TLC method to analyze gliclazide in its single component tablet formulation. Gliclazide were dissolved with chloroform. Gliclazide was chromatographed on silica Gel 60 F254 TLC plate using toluene: ethyl acetate in the ratio of 1:1 (v/v) as mobile phase. Gliclazide showed Rf value of 0.58 and was scanned at 234nm using Camag TLC Scanner 3. This method validation showed a good linearity with correlation coefficient (r) of 0.999 while the coefficient of variation of the regression function (Vx0) = 2.406%. Specificity showed calculation of purity and identity more than 0.99. The limit of detection (LOD) and the limit of quantification (LOQ) of the method was respectively 28.78 and 86.35 ng/spot respectively. The mean absolute recovery of Gliclazide from the simulation  sample was  100.5% ± 0.113 and the method precision was less than  5.3% whereas the mean of the recovery data was 100.3%. The proposed method has been applied to the determination of Gliclazide in commercial tablet formulations and the recovery of label claim were100.494%±0.348 for brand A and 100.111%±1.257% for brand B.  The developed method was successfully used for the assay of gliclazide. The method is simple, sensitive and precise; it can be used for the routine quality control testing of marketed formulations.DOI: http://dx.doi.org/10.3329/icpj.v1i10.11852 International Current Pharmaceutical Journal 2012, 1(10): 332-335

scholarly journals Determination of moxifloxacin hydrochloride in AVELOX pharmacological formulations using modified potentiometer sensors

Polimery ◽  
2021 ◽  
Vol 66 (11-12) ◽  
pp. 589-601
Author(s):  
Sachin Kumar ◽  
Sushil K. Sindhu ◽  
Praveen Kumar ◽  
Amit Sharma ◽  
Suresh Sagadevan
Keyword(s):  
Limit Of Detection ◽  
Modified Electrodes ◽  
Phosphomolybdic Acid ◽  
Official Method ◽  
Carbon Paste ◽  
Limit Of Quantification ◽  
Highly Sensitive ◽  
Electrode Sensor ◽  
Ph Range

Three different carbon paste (CP), silk-screen (SP) and poly (vinyl chloride) (PVC) modified electrodes were obtained to verify the reliability of AVELOX, the generic name of which is Moxifloxacin HCl (AV-MOXH). The sensing membranes were containing AVELOX ion associated complexes with sodium tetraphenylborate (NaTPB), phosphomolybdic acid (PMA), phosphotungstic acid (PTA), and ammonium reineckate (RN) as electroactive materials. All three electrodes gave fast, viable, and near-Nernstian linear responses over a relative wide concentration range that ranged from 1.010-6 to 1.010-2 mol / L AV-MOXH at 25° C with a monovalent cationic decrease. The sensors demonstrated a good discernment of AV-MOXH from numerous inorganic and organic compounds such as glucose, sucrose, Na+, Ca+, etc. Additionally, the isothermal coefficients along with selectivity coefficients were calculated. The modified Screen Printed Electrode sensor appeared to be highly sensitive for the determination of AV-MOXH. The electrode response was observed in pH range 2--6 for ISPE electrodes and IPVC electrodes and 3--7 for ICPE electrodes under various temperature conditions. The short response time, lifetime validity, recovery, and all the methods of validation such as limit of detection and limit of quantification were estimated. The potentiometric method turned out to be suitable for determining AV-MOXH in pharmacological formulations, and the findings obtained are comparable to the “HPLC official method” in terms of the agreement. As a result, the postulated potentiometric approach was verified in accordance with IUPAC guidelines.

scholarly journals Simultaneous determination of chloramphenicol and hydrocortisone acetate in cream using TLC desitrometry method

2012 ◽  
Vol 2 (1) ◽  
pp. 7-10 ◽  
Author(s):  
Nia Kristiningrum ◽  
Mia Rakhmawati
Keyword(s):  
Quality Control ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Pharmaceutical Journal ◽  
Hydrocortisone Acetate ◽  
Limit Of Quantification ◽  
Quality Control Testing ◽  
Label Claim ◽  
Routine Quality Control

A rapid and reproducible TLC method was developed for the determination of hydrocortisone acetate and chloramphenicol in cream. The analytes were dissolved with methanol and chromatographed on silica Gel GF 254 TLC plate using chloroform:ethyl acetate in the ratio of 1:1.5 (v/v) as mobile phase. Spots at Rf 0.29 and Rf 0.59 were recognized as chloramphenicol and hydrocortisone acetate, respectively. Quantitative analysis was done through densitometric measurement at wavelength 265 nm. Method was found linear over the concentration range of 300-900 ng/spot with the correlation coefficient of 0.999 and 0.998 for hydrocortisone acetate and chloramphenicol, respectively. Specificity showed calculation of purity and identity more than 0.99. The limit of detection (LOD) and the limit of quantification (LOQ) of the method were 23.84 and 71.51 ng/spot for hydrocortisone acetate, 21.06 and 63.18 ng/spot for chloramphenicol. The precision of this method was less than 2.8% whereas the means of the recovery data were 100.40± 0.579% for hydrocortisone acetate and 100.24±1.20% for chloramphenicol. The proposed method has been applied to the determination of hydrocortisone acetate and chloramphenicol in commercial cream formulations and the recovery of label claim were 99.23±0.66% (chloramphenicol) and 99.25±0.41% (hydrocortisone acetate) for brand A and 100.32±0.87% (chloramphenicol) and 100.53±0.78% (hydrocortisone acetate) for brand B. The developed method was successfully used for the assay of hydrocortisone acetate and chloramphenicol. The method is simple, sensitive and precise; it can be used for the routine quality control testing of marketed formulations.DOI: http://dx.doi.org/10.3329/icpj.v2i1.12871 International Current Pharmaceutical Journal 2012, 2(1): 7-10 

scholarly journals Development and validation of pimavanserin tartrate by normal phase- HPTLC method

2021 ◽  
Vol 8 (2) ◽  
pp. 75-78
Author(s):  
Mohammad Mojeeb Gulzar Khan ◽  
Pawar Vivek Laxman ◽  
Abdul Talib ◽  
Sandip Dinkar Firke ◽  
Mohan G Kalaskar ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Normal Phase ◽  
Limit Of Quantification ◽  
Label Claim ◽  
Development And Validation ◽  
Layer Chromatography ◽  
Hptlc Method

For the determination of pimvanserin tartrate in bulk and formulation, a rapid and simple High Performance Thin Layer Chromatography at 226 nm was developed and validated. The determination was carried out on thin coated aluminum backing plates covered with 200 mm layer of silica gel G 60 F254 (10×10 cm) plate as stationary phase and using a mobile phase of methanol: chloroform: trimethylamine (4:6:0.1 v/v/v) respectively. With a correlation coefficient (r) of 0.998, the development of pimvanserin tartrate was linear in the range of 0.7 to 4.2 µg/ml. The limit of detection (LOD) was found to be 7.68 ng/spot while the limit of quantification was found to be 23.28 ng/spot. The percentage label claim of pimvanserin tartrate in bulk and formulation was found to be 99 – 101 %. The percentage found in the formulation shows that no effect of excipient on drug. The conducted procedure has the benefit of being simple and quick. As a result, it can be used to examine pimvanserin tartrate in pharmaceutical formulations.

scholarly journals DETERMINATION OF INULIN FROM MULTIVITAMIN SYRUP PRODUCT BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY WITH RI DETECTOR

2012 ◽  
Vol 12 (2) ◽  
pp. 201-205 ◽  
Author(s):  
Yuni Retnaningtyas
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Regression Function ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Label Claim

At present, inulin is often added to multivitamin syrup product. The determination of the component of preparation both qualitatively and quantitatively is important to ensure quality of the product. This research is aimed to develop a high performance liquid chromatography method to analyze inulin in multivitamin syrup preparation. Separation of inulin from the sample, was performed using Aminex column HPX-87H (300 x 7.8 mm) Ion Exclusion at a temperature of 80 °C with isocratic elution system using deionized water as mobile phase at a flow rate of 0.5 mL/min, and detected by using refractive index detector. This method validation showed a good linearity with correlation coefficient (r) of 0.999 while the coefficient of variation of the regression function (Vx0) was 2.00%. The limit of detection (LOD) and the limit of quantification (LOQ) of the method were respectively 0.12 mg/mL and 0.37 mg/mL. The mean absolute recovery of inulin from the simulation sample was 99.42% and the method precision was less than 2%. The proposed method has been applied to the determination of inulin in commercial multivitamin syrup and the recovery of label claim was 99.9 mg/100 mL. The proposed HPLC method is rapid, simple, and selective for routine analysis.

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.

scholarly journals A novel LC-MS method development and validation for the determination of phenyl vinyl sulfone in eletriptan hydrobromide

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Indhu Priya Mabbu ◽  
G. Sumathi ◽  
N. Devanna
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Vinyl Sulfone ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Pressure Chemical Ionization ◽  
Pressure Chemical ◽  
Development And Validation ◽  
Phenyl Vinyl

Abstract Background The aim of the present method is to develop and validate a specific, sensitive, precise, and accurate liquid chromatography-mass spectrometry (LC-MS) method for the estimation of the phenyl vinyl sulfone in the eletriptan hydrobromide. The effective separation of the phenyl vinyl sulfone was achieved by the Symmetry C18 (50 × 4.6 mm, 3.5 μm) column and a mobile phase composition of 0.1%v/v ammonia buffer to methanol (5:95 v/v), using 0.45 ml/min flow rate and 20 μl of injection volume, with methanol used as diluent. The phenyl vinyl sulfone was monitored on atomic pressure chemical ionization mode mass spectrometer with positive polarity mode. Results The retention time of phenyl vinyl sulfone was found at 2.13 min. The limit of detection (LOD) and limit of quantification (LOQ) were observed at 1.43 ppm and 4.77 ppm concentration respectively; the linear range was found in the concentration ranges from 4.77 to 27.00 ppm with regression coefficient of 0.9990 and accuracy in the range of 97.50–102.10%. The percentage relative standard deviation (% RSD) for six replicates said to be injections were less than 10%. Conclusion The proposed method was validated successfully as per ICH guidelines. Hence, this is employed for the determination of phenyl vinyl sulfone in the eletriptan hydrobromide.

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