scholarly journals Penentuan Kadar Kalium Sorbat dan Persen Recovery Pada Selai dengan Metoda High Performance Liquid Chromatography

Author(s):  
Pevi Riani ◽  
Ulvie Ameinda Fannin

Fruit jam is one of the preserved products that have a soft texture that contains crushed fruit and is mixed with sugar with the addition or without the addition of water. Preservatives are added to prevent damage to jams. A preservative that is usually added to jam is potassium sorbate. Potassium sorbate is commonly used as a preservative because it dissolves more easily when added to food. This study aims to determine the levels of potassium sorbate in jam samples. Potassium sorbate was determined using High Performance Liquid Chromatography (HPLC). From the test results, it was found that potassium sorbate levels ranged from719, 65 mg/kg to 757,24 mg/kg. The results of this test will be compared with the standards set by the Food and Drug Supervisory Agency (BPOM) No. 36 of 2013 concerning the maximum limit for the use of preservative food additives, namely 500 mg/kg. From the test results, it can be seen that the potassium sorbate in all samples exceeds the quality standard set by the BPOM. Therefore, people must be more careful in choosing jam to consume daily. The test results have used the right method, namely by adjusting the stationary phase, mobile phase and the right wavelength so that the% recovery results are 103%.

2020 ◽  
Vol 103 (3) ◽  
pp. 779-783
Author(s):  
Özlem Aksu Dönmez ◽  
Şule Dinç-Zor ◽  
Bürge Aşçı ◽  
Abdürrezzak E Bozdoğan

Abstract Background In many countries, the levels of synthetic food additives causing harm to humans have been determined and their use has been controlled by legal regulations. Sensitive, accurate and low-cost analysis methods are required for food additive determination. Objective In this study, a fast high performance liquid chromatography-diode array detection (HPLC-DAD) analytical methodology for quantification of sodium benzoate, potassium sorbate, ponceau 4R, and carmoisine in a beverage was proposed. Methods Partial least squares (PLS) and principal component regression (PCR) multivariate calibration methods applied to chromatograms with overlapped peaks were used to establish a green and smart method with short isocratic elution. A series of synthetic solutions including different concentrations of analytes were used to test the prediction ability of the developed methods. Conclusions The average recoveries for all target analytes were in the range of 98.27–101.37% with average relative prediction errors of less than 3%. The proposed chemometrics-assisted HPLC-DAD methods were implemented to a beverage successfully. Analysis results from sodium benzoate, potassium sorbate, ponceau 4R, and carmoisine in a beverage by PLS-2 and PCR were statistically compared with conventional HPLC. Highlights The HPLC methods coupled with the PLS-2 and PCR algorithm could provide a simple, quick and accurate strategy for simultaneous determination of sodium benzoate, potassium sorbate, ponceau 4R, and carmoisine in a beverage sample.


2021 ◽  
Vol 1 ◽  
pp. 943-952
Author(s):  
Diana Safitri ◽  
W Wirasti ◽  
Khusna Santika Rahmasari ◽  
S Slamet

AbstractPotassium sorbate is one type of preservative that is often added in soft drinks. The addition is to inhibit and prevent the process of fermentation, acidification or other forms of destruction, or is an ingredient that can protect food from spoilage. The purpose of this study was to analyze the content of potassium preservatives in soft drink samples and to determine whether the levels of potassium sorbate in soft drinks were in accordance with the standards set by BPOM RI Number 36 of 2013 concerning the maximum limit for the use of food additives potassium sorbate which is 25 mg /kg body weight. The methods used in this research are qualitative and quantitative methods. The qualitative analysis used is the Color Test Method. The quantitative analysis used is High Performance Liquid Chromatography (HPLC) with methanol acetonitril as the mobile phase. The results obtained from the color test of the sample change the color of the sample to pink according to the comparison color while the HPLC results obtained that the sample content is calculated in each total volume, namely M1 = 0.051 mg/kg BW, M2 = 0.226 mg/kg BW, M3 = 0.209 mg/kg BW, M4 = 0.103 mg/kg BW, M5 = 0.322 mg/kg BW, M6 = 0.150 mg/kg BW, M7 = 0.173 mg/kg BW, M8 = 0.127 mg/kg BW, M9 = 0.195 mg /kg BW, M10 = 0.185 mg/kg BW, M11 = 0.107 mg/kg BW and M12 = 0.174 mg/kg BW. It can be said that samples M1 to M12 meet the requirements for potassium sorbate levels set by BPOM RI Number 36 of 2013.Keywords: soft drinks, potassium sorbate, preservatives, content analysis, HPLC. AbstrakKalium sorbat adalah salah satu jenis zat pengawet yang sering ditambahkan dalam minuman ringan. Penambahan tersebut untuk menghambat dan mencegah proses fermentasi, pengasaman atau bentuk perusakan lainnya, atau merupakan bahan yang dapat melindungi pangan dari pembusukan. Tujuan dari penelitian ini adalah untuk menganalisis kandungan pengawet kalium sorbatdalam sampel minuman ringan dan untuk mengetahui apakah kadar kalium sorbatdalam minuman ringan sudah sesuai dengan standar yang telah ditetapkan oleh BPOM RI Nomor 36 Tahun 2013 tentang batas maksimal penggunaan bahan tambahan pangan kalium sorbatyaitu sebesar 25mg/kg berat badan. Metode yang digunakan pada penelitian ini adalah metode kualitatif dan kuantitatif. Analisis kualitatif yang digunakan yaitu Metode Uji Warna. Analisis kuantitatif yang digunakan yaitu High Performance Liquid Chromatography (HPLC) dengan fase gerak metanol asetonitril. Hasil yang diperoleh dari uji warna terjadi perubahan warna sampel menjadi berwarna merah muda sesuai dengan warna pembanding sedangkan dengan hasil HPLC diperoleh kadar sampel yang dihitung dalam tiap jumlah total volume sampel yaitu M1 = 0,051 mg/kg BB, M2 = 0,226 mg/kg BB, M3 = 0,209 mg/kg BB, M4 = 0,103 mg/kg BB, M5 = 0,322 mg/kg BB, M6 = 0,150 mg/kg BB, M7 = 0,173 mg/kg BB, M8 = 0,127 mg/kg BB, M9 = 0,195 mg/kg BB, M10 = 0,185 mg/kg BB, M11 = 0,107 mg/kg BB dan M12 = 0,174 mg/kg BB. Dapat disimpulkan bahwa sampel M1 sampai M12 memenuhi persyaratan kadar kalium sorbatyang ditetapkan oleh BPOM RI Nomor 36 Tahun 2013.Kata Kunci: minuman ringan, kalium sorbat, pengawet, analisis kadar, HPLC.  


2019 ◽  
Vol 16 ◽  
Author(s):  
Joanna Wittckind Manoel ◽  
Camila Ferrazza Alves Giordani ◽  
Livia Maronesi Bueno ◽  
Sarah Chagas Campanharo ◽  
Elfrides Eva Sherman Schapoval ◽  
...  

Introduction: Impurity analysis is an important step in the quality control of pharmaceutical ingredients and final product. Impurities can arise from drug synthesis or excipients and even at small concentrations may affect product efficacy and safety. In this work two methods using high performance liquid chromatography (HPLC) were developed and validated for the evaluation of besifloxacin and its impurity synthesis, with isocratic elution and another with gradient elution. Method: The analysis by HPLC in isocratic elution mode was performed using a cyano column maintained at 25 °C. The mobile phase was composed by 0.5% triethylamine (pH 3.0): acetonitrile (88:12 v/v) eluted at a flow rate of 1.0 ml/min with detection at 330 nm. The gradient elution method was carried out with the same column and mobile phase components only modifying the rate between organic and aqueous phase during analysis. The procedures have been validated according to internationally accepted guidelines, observing results within acceptable limits. Results: The methods presented were found to be linear in the 140 to 260 µg/ml range for besifloxacin and 0.3 to 2.3 µg/ml for an impurity named A. The limits of detection and quantification were respectively 0.07 and 0.3 µg/ml for impurity A, with a 20 µL injection volume. The precision achieved for all analyses performed provided RSD inter-day equal to 6.47 and 6.36% for impurity A with isocratic elution and gradient, respectively. The accuracy was higher than 99% and robustness exhibited satisfactory results. In the isocratic method an analysis time of 25 min and 15 min was obtained for gradient. For impurity A, the number of theoretical plates in the isocratic mode was about 5000 while in the gradient mode it was about 45000, hence, it made the column more efficient by changing the mobile phase composition during elution. In besifloxacin raw material and in pharmaceutical product used in this study, other related impurities were present but but impurity A was searched for and not detected Conclusion: The proposed methods can be applied for quantitative determination of impurities in the analysis of the besifloxacin raw material, as well as in ophthalmic suspension of the drug, considering the quantitation limit.


1994 ◽  
Vol 59 (3) ◽  
pp. 569-574 ◽  
Author(s):  
Josef Královský ◽  
Marta Kalhousová ◽  
Petr Šlosar

The reversed-phase high-performance liquid chromatography of some selected, industrially important aromatic sulfones has been investigated. The chromatographic behaviour of three groups of aromatic sulfones has been studied. The optimum conditions of separation and UV spectra of the sulfones and some of their hydroxy and benzyloxy derivatives are presented. The dependences of capacity factors vs methanol content in mobile phase are mentioned. The results obtained have been applied to the quantitative analysis of different technical-grade samples and isomer mixtures. For all the separation methods mentioned the concentration ranges of linear calibration curves have been determined.


1977 ◽  
Vol 23 (12) ◽  
pp. 2288-2291 ◽  
Author(s):  
P H Culbreth ◽  
I W Duncan ◽  
C A Burtis

Abstract We used paired-ion high-performance liquid chromatography to determine the 4-nitrophenol content of 4-nitrophenyl phosphate, a substrate for alkaline phosphatase analysis. This was done on a reversed-phase column with a mobile phase of methanol/water, 45/55 by vol, containing 3 ml of tetrabutylammonium phosphate reagent per 200 ml of solvent. At a flow rate of 1 ml/min, 4-nitrophenol was eluted at 9 min and monitored at 404 nm; 4-nitrophenyl phosphate was eluted at 5 min and could be monitored at 311 nm. Samples of 4-nitrophenyl phosphate obtained from several sources contained 0.3 to 7.8 mole of 4-nitrophenol per mole of 4-nitrophenyl phosphate.


2021 ◽  
Vol 66 (3) ◽  
pp. 172-176
Author(s):  
Lyubov Borisovna Kalikova ◽  
E. R. Boyko

Adenine nucleotides (ATP, ADP and AMP) play a central role in the regulation of metabolism and energy: they provide the energy balance of the cell, determine its redox state, act as allosteric effectors of a number of enzymes, modulate signaling and transcription factors and activate oxidation or biosynthesis substrates. A large number of methods have been developed to determine the level of ATP, ADP and AMP, but the most universal and effective method for the separation and analysis of complex mixtures is the reversed-phase high-performance liquid chromatography method (RP-HPLC). The aim of this study is to determine the optimal conditions for the qualitative separation and quantitative determination of standard solutions of ATP (1 mmol/l), ADP (0,5 mmol/l) and AMP (0,1 mmol/l) by RP-HPLC. The degree of separation of adenine nucleotides was estimated by the time of peak output in the chromatogram. To achieve the goal, the following tasks were set: assess the effect of the temperature of the analysis on the separation and change of the release time of the analytes in the chromatogram; determine the most optimal composition of the mobile phase for the separation of ATP, ADP and AMP in the chromatogram (the content of the organic solvent in the solution); to identify the effect of pH of the mobile phase on the separation of standard solutions of adenine nucleotides; set the optimal molarity of the mobile phase for the separation of ATP, ADP and AMP in the chromatogram. It was found that the temperature of the analysis does not affect the quality of peak separation, while the composition and pH of the mobile phase have a significant effect on the complete and clear separation of the studied nucleotides in the chromatogram. It was determined that the analysis temperature of 37°C and the mobile phase of 0.05 M KH2PO4 (pH 6.0) are optimal for separating the peaks of adenine nucleotides.


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