Development and Validation of an UV-Visible Method for the Determination of β-Carotene in the Leafy Vegetables in Thailand

2014 ◽  
Vol 1033-1034 ◽  
pp. 652-657
Author(s):  
Napaporn Rattanat ◽  
Kanjana Yodmora

Determination of β-carotene content in four types of leafy vegetables, water morning glory, kale, lettuce and Chinese cabbage by using a simple, rapid and low cost of UV-Visible method. This study was in the concentration range of 0.5 to 12 mg/L, and showed the linear regression equation y = 0.0764x - 0.0008, and an excellent linearity with correlation coefficient (R2) was 0.9999. The accuracy of the method analysis was reported by percentage recovery of about 80-106%. The precision was reported by percent of relative standard deviation and varies for intra-day 3.92% and inter-day 3.99%. The limits of detection and limit of quantification were 0.004 and 0.013 mg/L, respectively. Acetone is the most suitable for extraction, ratio of weight of samples to solvent, and extraction time was 1:3 g/mL and 10 min. Moreover, the most appropriate storage temperature for leafy vegetable samples is 4°C. Evaluation of β-carotene content under the suitable conditions in the kale, Chinese cabbage, lettuce and water morning glory was found to be 27.96 ± 2.99, 19.35 ± 1.92, 18.78 ± 0.88 and 18.48 ± 1.86 mg/100 g, respectively.

2013 ◽  
Vol 829 ◽  
pp. 825-830 ◽  
Author(s):  
Ali Mazloomifar ◽  
Nafiseh Khatibi

The liquid-phase microextraction based on solidification of floating organic microdrop coupled with UV-visible spectrophotometer for preconcentration and determination of lead in the aqueous samples has been developed. In this technique, 20μL of 1-undecanol containing dithizone as the chelating agent (10-3mol L-1) was transferred to the water samples containing lead ions, and the solution was stirred for 25 min. The sample vial was cooled in an ice bath for 5 min. The solidified extract was transferred into a conical vial where it melted immediately, and then the organic phase was analyzed by Nanodrop spectrophotometer. Factors that influence the extraction and complex formation, such as pH, concentration of dithizone, extraction time, effect of ionic strenght, temperature and stirring rate were optimized. Under the optimized conditions, a preconcentration factor of 356, detection limit of 0.006 μgL-1, limit of quantification 0.018 μgL-1and a good relative standard deviation of 2.1% were obtained. The procedure was applied to sea water, mineral water and well water.


2021 ◽  
Vol 4 (2) ◽  
pp. 1-7
Author(s):  
Irman Idrus ◽  
Sabda Wahab ◽  
Andi Fitrah Nugraha ◽  
Syaiful Bachri

South Konawe District at Southeast Sulawesi Province is a producer of agriculture such as Papaya fruit ranging from 1168 quintals each year. Papaya fruit contains β-carotene which plays an important role in the formation of vitamin A in the body. This research was conducted to determine the β-carotene content of papaya fruit by using variables planting method, fruitage, and fruit condition. The mashed fruit was extracted using n-hexane: acetone: ethanol (2: 1: 1) v/v, then separated from polar and non-polar solutions. Qualitative analysis was carried out using the Carr-Price method and quantitative analysis or determination of β-carotene levels using the UV-Visible spectrophotometric method λ = 452.0 nm. The qualitative test results showed that the papaya fruit in the papaya fruit obtained by cultivation and growing wild with each variable half-ripe, ripe, and not fresh papaya identified the presence of β-carotene. The results of quantitative analysis of β-carotene levels in cultivated papaya fruit were 1.76 μL, half-ripe 1.32 μL, and cultivated young papaya 1.22 μL. In wild ripe papaya 1.75 μL, wild half-ripe papaya 1.3 μL and wild young papaya 1.21 μL. There is an effect of each test parameter starting from the parameters of planting method, fruitage, and fruit condition on β-carotene content in papaya fruit.


1997 ◽  
Vol 80 (5) ◽  
pp. 1057-1064 ◽  
Author(s):  
Willy Schuep ◽  
Joseph Schierle

Abstract Two sample preparation procedures for determination of total β-carotene and (all-)-β-carotene were tested in a collaborative study involving 14 laboratories and using 4 commercial products containing supplemented or natural β-carotene. One assay used classical sample preparation, consisting of saponification, extraction, washing, and drying ofthe extract and redissolution of residue for liquid chromatography (LC). The other assay used simple extraction without saponification. LC conditions were left for the analysts to decide as long as aclear separation of lycopene and ϑ-carotene from Bcarotene was achieved. Mean contents of test samples ranged from 0.3 to 18 mg/100 g for total β-carotene and from 0.2 to 16 mg/100 g for (all-)-β-carotene. Repeatability relative standard deviations (RSDr)for total B-carotene ranged from 2.9 to 5.6% and relative reproducibility standard deviation (RSDR) ranged from 6.5 to 15%. Corresponding values for(all-)-β-carotene were 3.3-5.1 % for RSDr and 8.4- 14% for RSDR. Excluding the (Z)-isomers from uantitation of β-carotene can result in significant underestimation of the effective β-carotene content especially if the LC systems used is high quality.


2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Suraj R. Chaudhari ◽  
Atul A. Shirkhedkar

Abstract Background Chlorthalidone is a diuretic medicinal agent used to treat hypertension. Lowering hypertension results in the prevention of strokes, heart attacks and kidney-related problems. Results In this work, the spectrophotometric investigation was employed to examine the reaction between chlorthalidone and 1, 2-naphthoquinone-4-sulfonate. A reaction is performed at the alkaline environment (pH 9.2) and heated at a moderate temperature of 60 ± 1 °C using a water bath. The red colour product was produced, and it displayed a maximum absorbance at 440.50 nm. Further, the advancement of response conditions was explored by UV/visible spectrophotometer. The stoichiometric of the reaction was considered by using Job’s plot and the reaction mechanism of the proposed work was drawn. The established approach obeyed the calibration curve in the concentration range of 2–12 μg/mL with a regression coefficient superior to 0.994. The accuracy of the method, assessed by employing the % recovery, was in the range of 99.06–99.60% with the % relative standard deviation being less than 2%. The limit of detection and limit of quantification were 0.58 μg/mL and 1.72 μg/mL, respectively. Conclusion A UV/visible spectrophotometric investigation for the analysis of the chlorthalidone in the tablet matrix was successfully established and validated. The established investigation was found to be simple and accurate, and because of its ease of use, the proposed strategy could be applied for quality control investigation of chlorthalidone in pharmaceutical matrices.


2020 ◽  
Vol 16 (4) ◽  
pp. 428-435
Author(s):  
Ahmed F.A. Youssef ◽  
Yousry M. Issa ◽  
Kareem M. Nabil

Background: Simeprevir is one of the recently discovered drugs for treating hepatitis C which is one of the major diseases across the globe. Objective: The present study involves the development of a new and unique High-Performance Liquid Chromatography (HPLC) method using fluorescence detection for the determination of simeprevir (SIM) in human plasma. Methods: Two methods of extractions were tested, protein precipitation using acetonitrile and liquidliquid extraction. A 25 mM dipotassium hydrogen orthophosphate (pH 7.0)/ACN (50/50; v/v), was used as mobile phase and C18 reversed phase column as the stationary phase. The chromatographic conditions were optimized and the concentration of simeprevir was determined by using the fluorescence detector. Cyclobenzaprine was used as an internal standard. Results: Recovery of the assay method based on protein precipitation was up to 100%. Intra-day and inter-day accuracies range from 92.30 to 107.80%, with Relative Standard Deviation (RSD) range 1.65-8.02%. The present method was successfully applied to a pharmacokinetic study where SIM was administered as a single dose of 150 mg SIM/capsule (Olysio®) to healthy individuals. Conclusion: This method exhibits high sensitivity with a low limit of quantification 10 ng mL-1, good selectivity using fluorescence detection, wide linear application range 10-3000 ng mL-1, good recovery and highly precise and validation results. The developed method can be applied in routine analysis for real samples.


2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Indhu Priya Mabbu ◽  
G. Sumathi ◽  
N. Devanna

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.


Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 1837
Author(s):  
Harischandra Naik Rathod ◽  
Bheemanna Mallappa ◽  
Pallavi Malenahalli Sidramappa ◽  
Chandra Sekhara Reddy Vennapusa ◽  
Pavankumar Kamin ◽  
...  

A quick, sensitive, and reproducible analytical method for the determination of 77 multiclass pesticides and their metabolites in Capsicum and tomato by gas and liquid chromatography tandem mass spectrometry was standardized and validated. The limit of detection of 0.19 to 10.91 and limit of quantification of 0.63 to 36.34 µg·kg−1 for Capsicum and 0.10 to 9.55 µg·kg−1 (LOD) and 0.35 to 33.43 µg·kg−1 (LOQ) for tomato. The method involves extraction of sample with acetonitrile, purification by dispersive solid phase extraction using primary secondary amine and graphitized carbon black. The recoveries of all pesticides were in the range of 75 to 110% with a relative standard deviation of less than 20%. Similarly, the method precision was evaluated interms of repeatability (RSDr) and reproducibility (RSDwR) by spiking of mixed pesticides standards at 100 µg·kg−1 recorded anRSD of less than 20%. The matrix effect was acceptable and no significant variation was observed in both the matrices except for few pesticides. The estimated measurement uncertainty found acceptable for all the pesticides. This method found suitable for analysis of vegetable samples drawn from market and farm gates.


2017 ◽  
Vol 9 (5) ◽  
pp. 102
Author(s):  
Sukhjinder Kaur ◽  
Taranjit Kaur ◽  
Gurdeep Kaur ◽  
Shivani Verma

Objective: The aim of the present work was to develop a simple, rapid, accurate and economical UV-visible spectrophotometric method for the determination of hydroquinone (HQ) in its pure form, marketed formulation as well as in the prepared nanostructured lipid carrier (NLC) systems and to validate the developed method.Methods: HQ was estimated at UV maxima of 289.6 nm in pH 5.5 phosphate buffer using UV-Visible double beam spectrophotometer. Following the guidelines of the International Conference on Harmonization (ICH), the method was validated for various analytical parameters like linearity, precision, and accuracy robustness, ruggedness, limit of detection, quantification limit, and formulation analysis.Results: The obtained results of the analysis were validated statistically. Recovery studies were performed to confirm the accuracy of the proposed method. In the developed method, linearity over the concentration range of 5-40 μg/ml of HQ was observed with the correlation coefficient of 0.998 and found in good agreement with Beer Lambert’s law. The precision (intra-day and inter-day) of the method was found within official RCD limits (RSD<2%).Conclusion: The sensitivity of the method was assessed by determining the limit of detection and limit of quantification. It could be concluded from the results obtained that the purposed method for estimation of HQ in pure form, in the marketed ointment and in the prepared NLC-formulation was simple, rapid, accurate, precise and economical. It can be used successfully in the quality control of pharmaceutical formulations and for the routine laboratory analysis.


2012 ◽  
Vol 11 (1) ◽  
pp. 55-63 ◽  
Author(s):  
Maizbha Uddin Ahmed ◽  
Mohammad Safiqul Islam ◽  
Tasmin Ara Sultana ◽  
AGM Mostofa ◽  
Muhammad Shahdaat Bin Sayeed ◽  
...  

Azithromycin is an effective and well-known antimicrobial agent. In the present study, a simple, sensitive and specific LC/MS/MS method has been developed and validated for the quantification of Azithromycin in  human serum samples using Clarithromycin as internal standard. Azithromycin was extracted from biological matrix  by using solid phase extraction process. The chromatographic separation was performed on Luna C18 (3 ?, 2x150   mm) column with a mobile phase consisting of 35 mM ammonium acetate buffer (mobile phase-A) and acetonitrile  and methanol in ratio of 90:10 ( as mobile phase-B) at a flow rate of 0.25 mL/min. The method was validated over a  linear concentration range of 0.5?50.0 ng/mL and limit of quantification (LOQ) was 0.5 ng/mL with a coefficient of  correlation (r2) = 0.9998. The intra-day and inter-day precision expressed as relative standard deviation were 1.64% – 8.43% and 2.32% – 9.92%, respectively. The average recovery of azithromycin from serum was 98.11%. The method  was successfully applied to a pharmacokinetic study after oral administration of Azithromycin 200 mg/5 ml suspension in healthy Bangladeshi volunteers. DOI: http://dx.doi.org/10.3329/dujps.v11i1.12488 Dhaka Univ. J. Pharm. Sci. 11(1): 55-63, 2012 (June)


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