scholarly journals Development and Validation of HPLC Method for the Simultaneous Determination of Five Food Additives and Caffeine in Soft Drinks

2016 ◽  
Vol 2016 ◽  
pp. 1-8 ◽  
Author(s):  
Bürge Aşçı ◽  
Şule Dinç Zor ◽  
Özlem Aksu Dönmez

Box-Behnken design was applied to optimize high performance liquid chromatography (HPLC) conditions for the simultaneous determination of potassium sorbate, sodium benzoate, carmoisine, allura red, ponceau 4R, and caffeine in commercial soft drinks. The experimental variables chosen were pH (6.0–7.0), flow rate (1.0–1.4 mL/min), and mobile phase ratio (85–95% acetate buffer). Resolution values of all peak pairs were used as a response. Stationary phase was Inertsil OctaDecylSilane- (ODS-) 3V reverse phase column (250 × 4.6 mm, 5 μm) dimensions. The detection was performed at 230 nm. Optimal values were found 6.0 pH, 1.0 mL/min flow rate, and 95% mobile phase ratio for the method which was validated by calculating the linearity (r2>0.9962), accuracy (recoveries ≥ 95.75%), precision (intraday variation ≤ 1.923%, interday variation ≤ 1.950%), limits of detection (LODs), and limits of quantification (LOQs) parameters. LODs and LOQs for analytes were in the range of 0.10–0.19 μg/mL and 0.33–0.63 μg/mL, respectively. The proposed method was applied successfully for the simultaneous determination of the mixtures of five food additives and caffeine in soft drinks.

2011 ◽  
Vol 8 (1) ◽  
pp. 340-346 ◽  
Author(s):  
Rajesh M. Kashid ◽  
Santosh G. Singh ◽  
Shrawan Singh

A reversed phase HPLC method that allows the separation and simultaneous determination of the preservatives methyl paraben (M.P.) and propyl paraben (P.P.) is described. The separations were effected by using an initial mobile phase of water: acetonitrile (50:50) on Inertsil C18 to elute P.P. and M.P. The detector wavelength was set at 205 nm. Under these conditions, separation of the two components was achieved in less than 10 min. Analytical characteristics of the separation such as precision, specificity, linear range and reproducibility were evaluated. The developed method was applied for the determination of preservative M.P. and P.P. at concentration of 0.01 mg/mL and 0.1 mg/mL respectively. The method was successfully used for determining both compounds in sucralfate suspension.


Author(s):  
NOVALINA BR PURBA ◽  
ABDUL ROHMAN ◽  
SUDIBYO MARTONO

Objective: The objective of this study was to optimize high-performance liquid chromatography (HPLC) method for the determination of acid orange 7 (AO7) and sudan II (SII) in blusher product based on response surface methodology using box behnken design (BBD) approach. Methods: Some factors responsible for HPLC separation including column temperature, mobile phase composition, flow rate were optimized using BBD. The responses evaluated were peak area, retention time, and tailing factor. AO7 and SII in blusher product has different properties, therefore both analytes were analysed using C18 column (Thermo Synergy Gold 250 mm x 4.6 mm i.d.,5 µm) using Shimadzu LC 20AD chromatograph equipped with photo-diode array (PDA) detector at 300-650 nm. The mobile phase used was acetonitrile-water (1:1 v/v), and acetonitrile composition was optimized at 35-50% for separation AO7 (ACN1), and 80-90% for SII (ACN2), delivered at the flow rate of 0.9–1 ml/min, using column temperature at 30-40 °C. Results: BBD showed that separation of AO7 was influenced by the concentration of ACN1, flow rate and column temperature. These factors affected retention time, peak area, and tailing factor with peak area was the most significant. Tailing factor was not significantly affected by each factor, and retention time was slightly effected. Otherwise, Sudan II was affected by all these factors except ACN1. The optimal condition obtained based BBD was ACN1 43%, ACN2 90%, the flow rate of 0.9 ml/min and a column temperature of 40 °C. Conclusion: BBD can be used to get optimum condition for analysis of AO7 and SII in blusher product.


2013 ◽  
Vol 49 (3) ◽  
pp. 521-528 ◽  
Author(s):  
Viviane Benevenuti Silva ◽  
Angel Arturo Gaona Galdos ◽  
Cintia Maria Alves Mothe ◽  
Michele Bacchi Pallastrelli ◽  
Maria Segunda Aurora Prado ◽  
...  

A simple, rapid, economical and reliable high performance liquid chromatographic method has been developed and successfully applied in simultaneous determination of ethinyl estradiol and drospirenone in coated tablets. The HPLC method was performed on a LiChroCART® 100RP column (125x4 mm i.d., 5 µm) with acetonitrile:water 50:50 (v/v) as mobile phase, pumped at a flow rate of 1.0 mL.min-1. The fluorescence detection for ethinyl estradiol was made at λex= 280 nm and λem= 310 nm and a UV detection for drospirenone was made at 200 nm. The elution time for ethinyl estradiol and drospirenone were 4.0 and 5.7 min, respectively. The method was validated in accordance to USP 34 guidelines. The proposed HPLC method presented advantages over reported methods and is suitable for quality control assays of ethinyl estradiol and drospirenone in coated tablets.


2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Hina Shamshad ◽  
Agha Zeeshan Mirza

Abstract Background Present work describes a fast, simple, and sensitive procedure for the simultaneous determination of cetirizine in the presence of quinolones using diclofenac sodium as an internal standard. The present work was designed to analyze these compounds in pharmaceutical and clinical labs being economical for use. Results The mobile phase consisted of the simple composition of methanol, acetonitrile, and water in a ratio of 50:20:30 with a pH adjusted to 3.1 at a flow rate of 1 mL min−1. The UV detection was performed at 225 nm. The linearity was assessed over the range of 2.5–50 μg mL−1 for all drugs. The parameters such as accuracy, precision, linearity (>0.999), and sensitivity were satisfactory. Conclusion The method was equally applicable for formulation and human serum with recovery values between 95 and 105%. The results of the method were validated statistically according to ICH guidelines.


2021 ◽  
Vol 9 (3) ◽  
pp. 1081-1089
Author(s):  
Juthi Mirza ◽  
Masuda Sultana ◽  
Md. Esrafil ◽  
Shamoli Akter ◽  
Md. Jahangir Alam ◽  
...  

Caffeine is one of the commonly used food additives, which has unique flavor characteristics and bitter taste and used in soft drinks as flavor enhancer. An experimental study was designed to determine the concentration of caffeine in different brands of soft drinks and energy drinks available in Bangladesh by using HPLC. For chromatographic analysis, A Luna 5 C18 (2) 100A column (250×4.6 mm) was used at 37°C temperature at the wavelength of 272nm. Chromatographic separation was determined using buffer of sodium acetate and acetic acid with acetonitrile at a ratio of 80:20 (pH=4.0; flow rate of 1.0 ml/min). The results of this study showed that caffeine content in soft drinks ranged from 19.63 to 101.73 mg/100ml and highest concentration of caffeine found in brand 3 samples while lowest concentration found in brand 2 samples. Significantly higher concentration of caffeine (p<0.05) found in six soft drinks sample when compared to BSTI and FDA reference value except brand 2 sample (p>0.05). Quantification of caffeine in different brands of energy drink sample revealed that, four brand sample contained caffeine; among them brand 3 sample showed the highest levels of caffeine 295.86 mg/100ml and lowest amount found in brand 1 sample (101.74 mg/100ml). Concentration of Caffeine in soft and energy drinks exceeded the national and international standard recommended range hence this proposed HPLC method can be used for routine determination and control of caffeine content in different drinks.


2009 ◽  
Vol 92 (4) ◽  
pp. 1082-1088 ◽  
Author(s):  
Rashmin B Patel ◽  
Mrunali R Patel ◽  
Madhira B Shankar ◽  
Kashyap K Bhatt

Abstract This paper describes validated HPLC and HPTLC methods for simultaneous determination of alprazolam (ALP) and fluoxetine hydrochloride (FXT) in pure powder and formulation. The HPLC separation was achieved on a Nucleosil C8 column (150 mm length, 4.6 mm id, 5 m particle size) using acetonitrilephosphate buffer pH 5.5 (45 + 55, v/v) as the mobile phase at a flow rate of 1.0 mL/min at ambient temperature. The HPTLC separation was achieved on an aluminum-backed layer of silica gel 60F254 using acetonetolueneammonia (6.0 + 3.5 + 0.5, v/v/v) as the mobile phase. Quantification in the HPLC method was achieved with UV detection at 230 nm over the concentration range 414 g/mL for both drugs, with mean recovery of 99.95 0.38 and 99.85 0.56 for ALP and FXT, respectively. Quantification in the HPTLC method was achieved with UV detection at 230 nm over the concentration range of 4001400 ng/spot for both drugs, with mean recovery of 99.32 0.45 and 99.78 0.81 for ALP and FXT, respectively. These methods are simple, precise, and sensitive, and they are applicable for the simultaneous determination of ALP and FXT in pure powder and formulations.


2014 ◽  
Vol 2014 ◽  
pp. 1-11 ◽  
Author(s):  
Fatma Turak ◽  
Mithat Dinç ◽  
Öznur Dülger ◽  
Mahmure Ustun Özgür

Four simple, rapid, and accurate spectrophotometric methods were developed for the simultaneous determination of two food colorants, Carmoisine (E122) and Ponceau 4R (E124), in their binary mixtures and soft drinks. The first method is based on recording the first derivative curves and determining each component using the zero-crossing technique. The second method uses the first derivative of ratio spectra. The ratio spectra are obtained by dividing the absorption spectra of the binary mixture by that of one of the components. The third method, derivative differential procedure, is based on the measurement of difference absorptivities derivatized in first order of solution of drink samples in 0,1 N NaOH relative to that of an equimolar solution in 0,1 N HCl at wavelengths of 366 and 451 nm for Carmoisine and Ponceau 4R, respectively. The last method, based on the compensation method is presented for derivative spectrophotometric determination of E122 and E124 mixtures with overlapping spectra. By using ratios of the derivative maxima, the exact compensation of either component in the mixture can be achieved, followed by its determination. These proposed methods have been successfully applied to the binary mixtures and soft drinks and the results were statistically compared with the reference HPLC method (NMKL 130).


Author(s):  
SYED IBRAHIM BAJE ◽  
B. JYOTHI ◽  
N. MADHAVI

Objective: The objective of the present study was to develop and validate a novel reverse phase high performance liquid chromatographic (RP-HPLC) method, for simultaneous determination of ritonavir (RIT), ombitasvir (OMB) and paritaprevir (PAR) in bulk mixtures, and in tablets. Methods: Determination of the drugs ritonavir (RIT), ombitasvir (OMB), and paritaprevir (PAR), was carried out applying Hypersil BDS C18 column (250 mm X 4.6 mm i.e., 5 µm particle size), with photodiode array detector at λmax of 254 nm. The mobile phase applied for the current study composed of two solvents, i.e. A (0.01N % w/v potassium di-hydrogen orthophosphate buffer, pH 3.0 adjusted with dilute orthophosphoric acid) and B (acetonitrile). The mobile phase was pumped at a flow rate of 1.0 ml/min in the isocratic mode. The validation study with respect to specificity, linearity, precision, accuracy, and robustness, limit of detection (LOD) and limit of quantification (LOQ) was carried out employing the ICH guidelines. Results: Ritonavir, ombitasvir, and paritaprevir showed linearity of response between 12.5-75 μg/ml for ritonavir, 3.125-18.75 µg/ml for ombitasvir and 18.75–112.5 µg/ml for paritaprevir, with a correlation coefficient (R2) 0.999, 0.999,0.999 for RIT, OMB, and PAR respectively. The % recovery obtained was 99.82±0.14 % RIT, OMB 100.03±0.96 % and for 99.96±0.26 % PAR. The LOD and LOQ values for RIT, OMB, PAR were obtained to be 0.02, 0.019and0.02, µg/ml and 0.07, 0.06 and 0.07 µg/ml, respectively. The method also exhibits good robustness for different chromatographic conditions like wavelength, flow rate, mobile phase, and injection volume. Conclusion: The method was successfully employed, for the quantification of RIT, OMB, and PAR, in the quality control of in-house developed tablets, and can be applied for the industrial use.


2013 ◽  
Vol 781-784 ◽  
pp. 787-791 ◽  
Author(s):  
Ya Li Xing ◽  
Liang Wu Bi ◽  
Zhen Dong Zhao ◽  
Tian Juan Xia

A quick and accurate HPLC method has been developed for the simultaneous quantification of two bioactive triterpenes, ursolic acid and oleanolic acid in Paulownia leaves. The samples were analyzed on a Shim-pack ODS-CLC (M) (4.6 mm × 250 mm, 5 μm) column kept at 21 °C, using the methanol and aqueous phase containing 0.05%phosphoric acid with the volumetric ratio of 91.7:8.3 as the mobile phase at a flow rate of 0.6 mL/ min, and the detection wavelength was set at 210 nm. The method was validated and applied to the simultaneous quantification of the two triterpenes in Paulownia leaf extract. The standard curves were established in the range of 0.44 ~ 8.75 μg for oleanolic acid and 0.92 ~ 18.37 μg for ursolic acid. The contents of oleanolic acid and ursolic acid in leaves of Paulownia were determinated using the HPLC method and the contents were 3.87 mg/g and 13.61 mg/g, respectively.


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