scholarly journals Saccharin Extraction And Analysis Of Drug And Food Samples By Derivative Ultraviolet (UV) Spectrophotometry

2018 ◽  
Vol 18 (2) ◽  
pp. 85-96
Author(s):  
Sarwendah Ratnawati Hermanto ◽  
Roto Roto ◽  
Agus Kuncaka

Saccharin extraction and analysis of drug and food samples was investegated by spectrophotometry ultraviolet (uv) derivative method were studied. The saccharin extraction was carried out using solvent of ethanol/chloroform (2:8 v/v). The limit of detection (LOD) and limit of quantification (LOQ) of the proposed method were  0.50 ppm and 1.82 ppm for the second order and 0.47 ppm and 1.58 ppm for the fourth, while for the zero order were 2,75 ppm and 8,55 ppm. The calibration curve was linear in the concentration range from 20-100 ppm (R2= 0.996 for the second order and R2=0.997 for the fourth). The percent recovery of saccharin was in the range 95.20-104.40% for the second order and 97.20-102.40% for the fourth. The range of saccharin concentration (w/w) in drugs, candies and toothpaste for the fourth derivative were 1.39±0.02 mg/kg until 7.15±0.05 mg/kg, 0.21±0.01 mg/kg until 2.09±0.01 mg/kg, and 0.15±0.03 mg/kg until 0.63±0.04 mg/kg, respectively. 

2013 ◽  
Vol 2013 ◽  
pp. 1-5
Author(s):  
Neelkant Prasad ◽  
Roshan Issarani ◽  
Badri Prakash Nagori

A simple and sensitive ultraviolet spectrophotometric method for quantitative estimation of glipizide in presence of lipid turbidity is described to avoid false estimation due to diffraction by turbidity. UV detection was performed at 230 nm, 225 nm, and 235 nm, and the calibration curve was plotted between resultant of absorbance of [230 nm − (225 nm + 235 nm)/2] and concentration of analyte. The calibration curve was linear over the concentration range tested (1–20 μg/mL) with limit of detection of 0.27 μg/mL and limit of quantification of 0.82 μg/mL. Percent relative standard deviations and percent relative mean error, representing precision and accuracy, respectively, for clear as well as turbid solutions, were found to be within acceptable limits, that is, always less than 0.69 and 0.41, respectively, for clear solution and 0.65 and 0.47, respectively, for turbid solution. Conclusively, our method was successfully applied for the determination of glipizide in clear as well as turbid solutions, and it was found that the drug analyte in both types of solutions can be detected from the same calibration curve accurately and precisely and glipizide entrapped in the liposomes or in proliposomal matrix was not detected.


Author(s):  
Lien Le Thi ◽  
Anh Bach Thuy ◽  
Khanh Cao Cong ◽  
Ha Tran Nguyen ◽  
Hong Hao Le Thi ◽  
...  

The determination of crinamidine in dietary supplements content by mass spectrometry (GC-MS/MS) was developed and validated. The method was performed on the DB5MS column (30m x 0,25mm; 0,25 μm), in combination with the tandem mass spectrometry. The parameters of the method were evaluated for selectivity, calibration curve, accuracy, precision, limit of detection (LOD) and limit of quantification (LOQ). The calibration curve was highly linear (the coefficient of determination 0.9970) within the concentration range of 5ppm-50ppm. The recovery at three concentrations were above 90,1%. The limit of detection (LOD) and limit of quantification (LOQ) of the methods were 3 and 10 mg/kg, respectively. All obtained results were acceptable according to the AOAC for dietary supplements. The method was applied to analyze 34 samples in Hanoi.


2017 ◽  
Vol 9 (6) ◽  
pp. 75
Author(s):  
Ritesh Kumar ◽  
Amrish Chandra ◽  
Swati Gupta ◽  
Pawan Kumar Gautam

Objective: The objectives of the present research was to develop a simple, precise, economical, accurate, reproducible and sensitive method for the quantitative estimation of lafutidine in bulk and its pharmaceutical dosage forms by Ultra Violet (UV) absorption spectrophotometry.Methods: The method uses 0.1 N HCl, pH 1.20 as a solvent of choice for the quantitative estimation of lafutidine in bulk and its tablets dosage form by UV absorption spectrophotometry at a wavelength of 290 nm. The method was validated for parameters like linearity, range, precision, Limit of Detection (LOD), Limit of Quantification (LOQ), accuracy, recovery and stability of the analyte.Results: Lafutidine exhibited absorbance maxima at 290 nm in 0.1 N HCl, pH 1.20 solvent. The developed method was validated as per the ICH validation guidelines. Beer’s law was obeyed in range of 0-30 µg/ml with r2= 0.9997. The LOD and LOQ values of lafutidine were found to be 0.545 µg/ml and 1.654 µg/ml respectively. The mean % recovery for the developed method was found to be in the range of 99.25 to 99.45 % respectively for the marketed dosage forms. The developed method was also found to be robust.Conclusion: The developed method was found suitable for the routine quantitative analysis of lafutidinein bulk and pharmaceutical dosage form. It was also concluded that developed UV spectrophotometry method was accurate, precise, linear, reproducible, robust and sensitive.


INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (04) ◽  
pp. 38-46
Author(s):  
H Parimi ◽  
C Bolla ◽  
B. M. Gandhi ◽  
B. R Vatchavai ◽  
S. S Kamatham ◽  
...  

The main objective of the present work was to develop a simple, precise, accurate and reproducible UV-Spectrophotometric and stability indicating RP-HPLC methods for simultaneous estimation of moxifloxacin HCl (MOX) and ketorolac tromethamine (KET) in bulk and ophthalmic dosage forms. UV Spectrophotometry was carried out by simultaneous equation method using distilled water : acetonitrile (50:50 V/V) as solvent. The wavelengths were found to be 295 nm for MOX and 322 nm for KET. The isobestic point was found to be 308 nm. The linearity range is 2-10 μg/mL for both MOX and KET with correlation co-efficient >0.99. The separation of these two drugs using RP-HPLC was achieved on a SHISHEDO C18, 250×4.6 mm, 5 micron size column with a mobile phase consisting of acetonitrile and acetate buffer (45:55 V/V) at pH 4.0 at a flow rate of 1 mL/min and UV detection at 308 nm. The retention times were observed to be 2.418 and 3.827 minutes for MOX and KET, respectively. Linearity was found to be 10-50 μg/mL for both MOX and KET, respectively. The two developed methods were successfully validated for accuracy, precision, linearity, limit of detection, limit of quantification and robustness. The two developed methods were validated according to ICH guidelines and were found to be with in the limits. The stress testing of the drugs individually was carried out under acidic, alkaline, oxidation, photo-stability and thermal degradation conditions and its degradation products were studied. These two methods could be used for simultaneous estimation of MOX and KET in bulk and ophthalmic dosage forms.


2019 ◽  
Vol 10 (2) ◽  
pp. 1392-1396 ◽  
Author(s):  
Khalaf F Alsamarrai ◽  
Menaa Abdulsalam Al-Abbasi ◽  
Eman Thiab Alsamarrai

A new, sensitive, simple and cheap spectrophotometric method for the determination of Neomycin Sulphate (NEO) in pharmaceutical forms has been developed. The method is based on the reaction between NEO and NIN in basic medium. The maximum absorbance was at 574 nm. The conditions affecting the reaction were optimized. Under the optimal conditions, the calibration curve was linear over the range of 0.0002-0.0011 mol/L. The limit of detection and limit of quantification were 5.423×10-6 mol/L, and 1.643×10-5 mol/L, RSD% of seven replicate was 0.8217- 0.8321% and Rec% was between 99.2168-100.8857%. The proposed method was successfully applied to the determination of NEO tablets form.


2012 ◽  
Vol 2012 ◽  
pp. 1-4 ◽  
Author(s):  
Ajay Rana ◽  
Harsh Pratap Singh ◽  
Devendra Dhyani

Incarvillea emodi (Bignoniaceae) is a rich source of bioactive iridoid glucosides. This plant contains two major iridoid glucosides: plantarenaloside, a neurotropic compound, and boschnaloside, a strong antibacterial compound. Here, in this study we have developed a simple and fast HPLC-DAD method for the total comparative estimation of these two major iridoids from different parts of Incarvillea emodi. A linear calibration curve (r2=0.999) for both iridoid glucosides in varying range (15.6–500 μg/ml) is obtained. The limit of detection (LOD) and limit of quantification (LOQ) for plantarenaloside were 11.4 ng and 38 ng and for boschnaloside were 22.8 ng and 76 ng, respectively. The shoots, roots, and flowers of Incarvillea emodi have a combined presence of 7.66, 1.22, and 6.99 percent of these iridoid glucosides on dry weight basis. In shoots, plantarenaloside shows complete dominance (6.78%) over boschnaloside (0.88%), and a reversal of this trend was observed in case of flowers where boschnaloside shows complete dominance (6.12%) over plantarenaloside (0.87%). The roots contain 1.19% and 0.03% of both iridoids, respectively.


2018 ◽  
Vol 8 (5-s) ◽  
pp. 277-282 ◽  
Author(s):  
AK Jain ◽  
BK Dubey ◽  
D Basedia ◽  
S Dhakar ◽  
M Ahirwar ◽  
...  

An accurate, precise, sensitive and reproducible High-performance liquid chromatographic (HPLC) and UV spectrophotometric methods were developed and validated for the quantitative determination of haloperidol (HPD) in bulk drug and pharmaceutical formulation. Different analytical performance parameters such as linearity, precision, accuracy, specificity, limit of detection (LOD) and limit of quantification (LOQ) were determined according to International Conference on Harmonization ICH Q2B guidelines. The RP-HPLC method was developed by the isocratic technique on a reversed-phase Thermo C18 (250 × 4.6 mm, 5µm) column with mobile phase consisting of Methanol: Acetonitrile (50:50v/v) at flow rate of 1.0 ml/min. The retention time for HPD was 2.238±0.3min. The UV spectrophotometric determinations were performed at 244 nm using 80% methanol as a solvent. The linearity range for HPD was 5-25 μg/ml for both HPLC and UV method. The linearity of the calibration curves for each analyte in the desired concentration range was good (r2 >0.999) by both the HPLC and UV methods. The method showed good reproducibility and recovery with percent relative standard deviation less than 2%. Moreover, the accuracy and precision obtained with HPLC co-related well with the UV method which implied that UV spectroscopy can be a cheap, reliable and less time consuming alternative for chromatographic analysis. The proposed methods are highly sensitive, precise and accurate and hence successfully applied for determining the assay and in vitro dissolution of a marketed formulation. Keywords: HPLC, UV Spectrophotometry, Haloperidol, Pharmaceutical formulation, Method validation, Quantitative analysis


Foods ◽  
2020 ◽  
Vol 9 (5) ◽  
pp. 661 ◽  
Author(s):  
Sharaf S. Omar ◽  
Moawiya A. Haddad ◽  
Salvatore Parisi

Background: In Jordan as in other worldwide countries, mycotoxins are considered a serious national problem in food supplies. As a result, almost all nations are setting and adopting different regulations targeting the control of mycotoxins levels in the domestic food supply, including the problem of reliable sampling and analysis methods. Objective: It is necessary to improve and give evidence of analytical abilities of laboratories within Jordan and developing countries enabling them to monitor mycotoxins effectively in food to overcome non-tariff obstacles. Methods: We analyzed 40 samples from wheat, corn, dried fig and dried coffee beans for total aflatoxin content using High Pressure Liquid Chromatography (HPLC) and Enzyme Linked Immunesorbent Assay (ELISA) methods. Results: 40% of samples from wheat, 60% from corn, 30% from dried fig, and 50% from dried coffee beans were found positive when speaking of total aflatoxins, with average values between 1.14 and 4.12 μg/kg. Obtained results allow considering all tested food samples as fit for human consumption if compared with the labeled regulatory limit of allowed aflatoxins in the European Union. In detail, the limit of detection and the limit of quantification for methods used in this study were significantly lower than the maximum limits established by the European Union. Highlights: The procedure used in this study is suitable for detection of mycotoxins at very low concentration.


2015 ◽  
Vol 20 (2) ◽  
pp. 71-75
Author(s):  
Mareta Mukharbekovna Ibragimova ◽  
Latif Tulaganovich Ikramov

Objective: An increasing numbers of cases of poisonings by glimepiride, either attempted suicide or accidental, combined with the absence of reliable methods for the detection and quantitation of glimepiride in biological matrices is the basis for the need for the development of new analytical techniques for forensic analysis.Materials and Methods: Analyses were performed using drug- free biological fluids (whole blood and urine). Specimens were spiked with chromatographically pure glimepiride. After hydrolysis with diluted hydrochloric acid at 50-60 °C for 15-20 min and a double extraction into chloroform, glimepiride was identified by thin-layer chromatography. Standard solution of glimepiride (1 mg/mL) and Sorbfil chromatographic plates were used for thin-layer chromatography. The thin-layer chromatography studies showed that the best mobile phase was chloroform:acetone (9:1), Rf value of glimepiride in five examinations was 0.37±0.02. Visualization of glimepiride was achieved byspraying with Dragendorff’s, Bushard’s, or diphenylcarbazone-chloroform solution followed by mercuric sulphate. The limit of detection of pure glimepiride by thin-layer chromatography was 0.5 p/mL, 1.5 p g/mL in whole blood and 1.0 p g/mL in urine. For spectrophotometric determinations of glimepiride, a UV/VIS spectrophotometer with 1 cm matches quartz cell was used. Standard solutions of glimepiride in ethanol were prepared at concentrations of 1-50 p g/mL and scanned in full-scan mode between 200-400 nm.Results and Conclusion: The wavelength maxima for glimepiride was found to be 227 nm with molar absorptivity of 3.2685x10 4 l/mol/cm. Beer’s law was obeyed in the concentration range of 2-40 p g/mL. The limit of detection and limit of quantification were found to be 0.97 p g/mL and 2.70 p g/mL, respectively. The results have been successfully applied in blood of patients after oral administration and on postmortem blood in an overdose death.Keywords: Glimepiride, Thin-layer chromatography, Spectrophotometry.


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