• Journal of Food Hygiene and Safety
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• v.37 no.4
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• pp.216-224
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• 2022

This study was aimed at validating the analysis methods for deacetylasperulosidic acid (DAA), total sugar, galacturonic acid, glucose, and galactose, which are the indicator components of fermented Morinda citrifolia polysaccharide extract (Vitalbos). We modified the previously reported methods for validating the analytical methods. The specificity, linearity, precision, accuracy, limit of detection (LOD), and limit of quantification (LOQ) were measured using phenol-sulfuric acid method and high-performance liquid chromatography (HPLC). The retention time and spectrum of the standard solution of Vitalbos coincided, confirming the specificity. The calibration curve correlation coefficient (R²), of five indicator components, ranged from 0.9995-0.9998, indicating excellent linearity of 0.99 or more. The intra-day and inter-day precision range of the assay was 0.14-3.01%, indicating a precision of less than 5%. The recovery rate was in the range of 95.13-105.59%, presenting excellent accuracy. The LOD ranged from 0.39 to 0.84 ㎍/mL and the LOQ ranged from 1.18 to 2.55 ㎍/mL. Therefore, the analytical method was validated for DAA, total sugar, galacturonic acid, glucose, and galactose, in Vitalbos. The indicator component content in Vitalbos was determined using a validated method. The contents of DAA, total sugar, galacturonic acid, glucose, and galactose were 2.31±0.06, 475.92±5.95, 72.83±1.05, 71.63±2.44, and 67.30±2.31 mg/g of dry weight, respectively. These results suggest that the developed analytical method is efficient and could contribute to the quality control of Vitalbos, as a healthy functional food material.

• Analytical Science and Technology
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• v.22 no.5
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• pp.432-438
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• 2009

In order to develop the analytical method for the pharmaceutical tablets containing ranitidine HCl by square wave voltammetry (SWV), $5.00{\times}10^{-5}M$ ranitidine HCl solutions prepared with phosphate buffers of various pH values were investigated by SWV. The well defined main peak due to the electrochemical reduction of $-NO_2$ in the structure of ranitidine moved towards the cathodic direction by -70 mV/pH as the pH values were increased indicating the involvement of hydrogen in its reduction. The calibration curve, the plot of peak currents (Ip) vs. concentrations of ranitidine HCl in the range between $1.00{\times}10^{-7}M$ and $1.00{\times}10^{-5}M$ showed linearity with slopes of $232,530{\mu}A/M$ (pH 6.14), $289,015{\mu}A/M$ (pH 7.07) and $232,843{\mu}A/M$ (pH 8.01). When one pharmaceutical tablet was simply dissolved in the phosphate buffer with a pH value of 6.14 and determined by standard addition method using SWV, the within-day precision study (n=4) resulted in the contents of ranitidine HCl as $171{\pm}2.1mg$ ($102{\pm}1.3%$ of the specified contents, RSD of 1.2%) in a tablet of Curan$^{(R)}$. The inter-day precision for 5 days was 1.1% of RSD. For Zantac$^{(R)}$ the within-day precision study (n=4) showed the contents of ranitidine HCl as $167{\pm}0.8mg$ ($99{\pm}0.5%$ of the specified contents, RSD of 0.5%) in a tablet and the inter-day precision for 5 days was 0.3% of RSD.

• Analytical Science and Technology
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• v.36 no.6
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• pp.291-299
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• 2023

The benzo[a]pyrene in edible oils is extracted using methods such as Liquid-liquid, soxhlet and ultrasound-assisted extraction. However these extraction methods have significant drawbacks, such as long extraction time and large amount of solvent usage. To overcome these drawbacks, this study attempted to improve the current complex benzo[a]pyrene analysis method by applying the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method that can be analyzed in a simple and short time. The QuEChERS method applied in this study includes extraction of benzo[a]pyrene into n-hexane saturated acetonitrile and n-hexane. After extraction and distribution using magnesium sulfate and sodium chloride, benzo[a]pyrene is analyzed by liquid chromatography with fluorescence detector (LC/FLR). As a result of method validation of the new method, the limit of detection (LOD) and quantification (LOQ) were 0.02 ㎍/kg and 0.05 ㎍/kg, respectively. The calibration curves were constructed using five levels (0.1~10 ㎍/kg) and coefficient (R²) was above 0.99. Mean recovery ratio was ranged from 74.5 to 79.3 % with a relative standard deviation (RSD) between 0.52 to 1.58 %. The accuracy and precision were 72.6~79.4 % and 0.14~7.20 %, respectively. All results satisfied the criteria ranges requested in the Food Safety Evaluation Department guidelines (2016) and AOAC official method of analysis (2023). Therefore, the analysis method presented in this study was a relatively simple pretreatment method compared to the existing analysis method, which reduced the analysis time and solvent use to 92 % and 96 %, respectively.

• Korean Journal of Environmental Agriculture
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• v.32 no.3
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• pp.214-223
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• 2013

BACKGROUND: This study focused on the development of an analytical method about dichlorprop (DCPP; 2-(2,4-dichlorophenoxy)propionic acid) which is a plant growth regulator, a synthetic auxin for agricultural commodities. DCPP prevents falling of fruits during their growth periods. However, the overdose of DCPP caused the unwanted maturing time and reduce the safe storage period. If we take fruits with exceeding maximum residue limits, it could be harmful. Therefore, this study presented the analytical method of DCPP in agricultural commodities for the nation-wide pesticide residues monitoring program of the Ministry of Food and Drug Safety. METHODS AND RESULTS: We adopted the analytical method for DCPP in agricultural commodities by gas chromatograph in cooperated with Electron Capture Detector(ECD). Sample extraction and purification by ion-associated partition method were applied, then quantitation was done by GC/ECD with DB-17, a moderate polarity column under the temperature-rising condition with nitrogen as a carrier gas and split-less mode. Standard calibration curve presented linearity with the correlation coefficient ($r^2$) > 0.9998, analysed from 0.1 to 2.0 mg/L concentration. Limit of quantitation in agricultural commodities represents 0.05 mg/kg, and average recoveries ranged from 78.8 to 102.2%. The repeatability of measurements expressed as coefficient of variation (CV %) was less than 9.5% in 0.05, 0.10, and 0.50 mg/kg. CONCLUSION(S): Our newly improved analytical method for DCPP residues in agricultural commodities was applicable to the nation-wide pesticide residues monitoring program with the acceptable level of sensitivity, repeatability and reproducibility.

• Journal of Food Hygiene and Safety
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• v.34 no.3
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• pp.227-234
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• 2019

An analytical method was developed for the determination of oxytetracycline in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). After the samples were extracted with methanol, the extracts were adjusted to pH 4 by formic acid and sodium chloride was added to remove water. Dispersive solid phase extraction (d-SPE) cleanup was carried out using $MgSO_4$ (anhydrous magnesium sulfate), PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed with LC-MS/MS using ESI (electrospray ionization) in positive ion MRM (multiple reaction monitoring) mode. The matrix-matched calibration curves were constructed using six levels ($0.001{\sim}0.25{\mu}g/mL$) and coefficient of determination ($r^2$) was above 0.99. Recovery results at three concentrations (LOQ, $10{\times}LOQ$, and $50{\times}LOQ$, n=5) were from 80.0 to 108.2% with relative standard deviations (RSDs) less than of 11.4%. For inter-laboratory validation, the average recovery was in the range of 83.5~103.2% and the coefficient of variation (CV) was below 14.1%. All results satisfied the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for oxytetracycline determination in agricultural commodities. This study could be useful for safety management of oxytetracycline residues in agricultural products.