• Korean Journal of Pharmacognosy
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• v.53 no.3
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• pp.162-169
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• 2022

This study investigated the mycotoxins (aflatoxin B₁, B₂, G₁, G₂, fumonisin B₁, B₂, ochratoxin A and zearalenone) contained in edible and medicinal plants in Seoul Yangnyeong market during 2020-2021. We analyzed contamination of mycotoxins using LC-MS/MS and evaluated risk assessment. The method was validated by assessing matrix effects, linearity, limit of detection (LOD), limit of quantification(LOQ) and recovery. Matrix-matched standard calibration was used for calibration curves showed good linearity (r²>0.999). The LOD, LOQ and recovery were 0.01-0.23 ㎍/kg, 0.04-0.71 ㎍/kg and 75.5-117.9% respectively. Mycotoxins were detected in 22 of 171 samples; aflatoxin B₁ (6.66 ㎍/kg), fumonisin (7.54-64.68 ㎍/kg), ochratoxin A (4.21-10.56 ㎍/kg) and zearalenone (7.31-60.76 ㎍/kg). In the risk assessment, the MOE (Margine of Exposure) of aflatoxin B₁ and ochratoxin A were in the range of 1.48×10³-2.36×10⁵. No items exceeded 100% in %TDI (Tolerable Daily Intake) of fumonisin (B₁+B₂) and zearalenone.

• The Korean Journal of Food And Nutrition
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• v.36 no.2
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• pp.93-102
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• 2023

Centella asiatica (C. asiatica) has been widely used in food, cosmetics, and pharmaceutical industry as a functional material. In a previous study, we have investigated not only pharmacological effects such as antioxidative and anti-inflammatory effects, but also analyzed various functional ingredients. In this study, triterpenoids were analyzed using HPLC-DAD to determine marker compounds among functional ingredients. When triterpenoids were analyzed, asiaticoside from C. asiatica was determined as an optimal marker compound. Next, specificity, linearity, limited of detection (LOD), limited of quantification (LOQ), precision, accuracy, and range were evaluated using HPLC-DAD to determine asiaticoside contents in C. asiatica juice and extracts. The specificity was elucidated by chromatogram and retention time using an established analytical method. The coefficient of correlation obtained was 0.9996. LOD was 4.99 ㎍/mL and LOQ was 15.12 ㎍/mL. Intra- and inter-day precision of asiaticoside were determined to be 0.48~1.68% and 0.08~1.09%, respectively. Furthermore, the recovery rate of asiaticoside was 98.88% and the analytical range of Field-70E was determined to be 0.625~10 mg/mL. As a results of evaluating ABTS, DPPH, and FRAP antioxidative effect, Field-70E showed potent antioxidant activities. Results of this study could be used as basic data for quality standardization of C. astiatica juice and extracts.

• Analytical Science and Technology
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• v.26 no.2
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• pp.142-153
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• 2013

A new, rapid, and simple analytical method was developed and validated using high performance liquid chromatograph-photodiode array detector (HPLC-PAD) for the determination of lepimectin residues in agricultural commodities. The lepimectin residues in samples were extracted with methanol, partitioned with dichloromethane, and then purified with glass column filled with subsequently to aminopropyl ($NH_2$) solid phase extraction (SPE) cartridge. The purified samples were detected using HPLC-PAD. Correlation coefficient ($R^2$) of both lepimectin $A_3$ and $A_4$ solutions were 0.9999. The method was validated using cucumber spiked with lepimectin at 0.02 and 0.2 mg/kg and pepper, mandarin, hulled rice, potato, soybean at 0.02 and 0.5 mg/kg. Average recoveries were 76.0~114.8% with relative standard deviation less than 10%, and limit of detection (LOD) and limit of quantification (LOQ) were 0.005 and 0.01 mg/kg, respectively. The result of recoveries and overall coefficient of variation of a laboratory results in Gwangju regional KFDA and Daejeon regional KFDA was followed with Codex guideline (CAC/GL 40). Therefore, developed method in this study is accurate, rapid, and appropriate for lepimectin determination and will be used to keep safety of lepimectin residues in agricultural products.

• Journal of Food Hygiene and Safety
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• v.35 no.4
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• pp.398-410
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• 2020

In this study, the contents of soluble vitamins B₁ (thiamin), B₂ (riboflavin), and B₃ (niacin) in 13 kinds of rice, 11 kinds of noodles, and 15 kinds of sauces were identified. The limit of detection (LOD) and limit of quantification (LOQ) were checked to determine the reliability of the experimental results, and the accuracy of the results through the standard reference material (SRM 1849a) was verified to show excellent indicators. As for thiamin, japchaebab (stir-fried glass noodles with rice) was found to contain the highest content among rice dishes, makguksu (buckwheat noodles) among noodle dishes, and tomato spaghetti sauce among sauces. Riboflavin was identified as having the highest content in slightly spicy jajangbab (black-bean sauce with rice), bibimguksu (spicy noodles) for noodles, and spicy curry with turmeric for sauces. Niacin was highest in content in the deep and rich flavors of spicy chicken-fried rice, janchiguksu (banquet noodles), and black-bean sauce, respectively. As a result of checking the amount of recommended daily intake of water-soluble vitamins for Korean adult men and women, the highest content of riboflavin was 217.40% for men and 271.75% for women. Through this study, we are going to establish a database of nutrients for the water-soluble vitamins contained in rice, noodles, and sauces to provide the necessary dietary data concerning the content of the water-soluble vitamins contained in foods for daily recommended intake.

• Journal of Food Hygiene and Safety
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• v.31 no.5
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• pp.311-318
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• 2016

Azorubine is a synthetic tar color containing azo-bond in the molecular structure. This food colorant has been allowed to be used for beverages, cheese and dried fruits in the European Union and for some food in Australia. Even though it is applicable as a food color in many countries, this compound has not been permitted in Korea so far as a food additive. Thus, this study was performed to establish an analysis method for azorubine in Korea by comparison of three HPLC analysis methods for azorubine and other azo-compounds which are officially used in the European Food Safety Authority (EFSA, EU), the Food Standard Agency (FSA, England) and the National Institute of Food and Drug Safety Evaluation (NIFDS, Korea). The analysis method of the FSA for azorubine showed the best linearity ($r^2=0.999$), limit of detection (LOD, $0.07{\mu}g/mL$), limit of quantification (LOQ, $0.20{\mu}g/mL$), precision (0~0.5%) and accuracy (98.6~100.7%) among tested HPLC methods using a C-18 column and diode array detector (DAD) with ammonium acetate solution and acetonitrile as an eluent solution. Finally selected method of FSA was further verified by inter-day and intra-day experiments with linearity, LOD, LOQ, precision and accuracy. Recovery test showed the recover ratios of 97~103%, 95~101%, and 93~102% in beverages, breads/snacks and other foods, respectively. Inter-laboratory test represented the absolute value of z-score of less than 2 which means satisfactory levels in this test. Selected method of FSA showed reliable analytical results in application test using food samples collected in commercial markets in Europe.

• Journal of Food Hygiene and Safety
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• v.32 no.5
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• pp.418-423
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• 2017

An analytical method for the determination of dexamethasone (DM) in bovine milk samples was developed and validated using liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). Milk samples were extracted by the liquid-liquid extraction based on acetonitrile. The chromatographic separation was achieved on a reverse phase $C_{18}$ column with gradient elution using a mobile phase of 0.1% formic acid in 95% acetonitrile. The procedure was validated according to the Ministry of Food and Drug Safety guideline determining accuracy, precision, limit of detection (LOD), and limit of quantification (LOQ). Mean recoveries of DM from spiked milk samples (25, 125, and 1,250 ng/mL) were 98.9-109.6%, and the relative standard deviation was between 1.7 and 4.4%. Linearity in concentration range of 12.5-1,250 ng/mL was obtained with the correlation coefficient ($r^2$) of 0.9997. LOD and LOQ for the investigated DM were 0.15 and 0.5 ng/mL depending on milk samples, respectively. This method was reliable, sensitive, economical and suitable for routine monitoring of DM residues in bovine milk.

• Journal of Food Hygiene and Safety
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• v.34 no.4
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• pp.334-339
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• 2019

A procedure based on high-performance liquid chromatography (HPLC) is described to determine ${\beta}-carotene$ in infant formulas. The method for ${\beta}-carotene$ analysis was performed on a C18 reversed-phase column using acetonitrile/methanol/dichloromethane (6:1:3, v/v/v) as a mobile phase. ${\beta}-Carotene$ was determined in HPLC with photo diode array (PDA) detector. The parameters of validation were specificity, linearity, LOD, LOQ, accuracy, precision and repeatability. The specificity was confirmed by the retention time and the linearity ($R^2$), which was over 0.999 in the range of 0.125~2 mg/L. The detection and quantification limits were 0.064 and 0.193 mg/L, respectively. The accuracy and precision of this method using an STD spiked sample were 80~119% and 1.02~2.05% respectively. The method was applied to the analysis of various infant formula and follow-up formulas products containing ${\beta}-carotene$, and all the products contained acceptable levels of ${\beta}-carotene$ for nutrition labeling.

• Korean Journal of Pharmacognosy
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• v.45 no.4
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• pp.338-345
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• 2014

HPL-4 is a new herbal formulation developed for the treatment of osteoarthritis. In this study, we took HPL-4 to develop a method for simultaneous determination of nine marker compounds (protocatechuic acid, chlorogenic acid, liriodendrin, nodakenin, ${\beta}$-$\small{D}$-(3-O-sinapoyl)frucofuranosyl-${\alpha}$-$\small{D}$-(6-O-sinapoyl)glucopyranoside, quercitrin, 6-gingerol, decursin and decursinol angelate) present in the formulation. The analytes were separated by UPLC system consisting of diode array detector at 205 nm and RP-amide column, and solvent system of $ACN/0.1%H_3PO_4$. Analytical method was validated to evaluate its linearity, limit of detection (LOD), limit of quantification (LOQ), precision, and accuracy. All standards showed good linearity ($R^2$ >0.99) in the rage of $0.25-400.0{\mu}g/mL$. The LOD and LOQ were within the range of 0.021-0.148 and $0.070-0.448{\mu}g/mL$, respectively. Intra- and inter-day precision was less than RSD 4.0% and the accuracy was range from 92.00-104.81% with RSD<4.2%. The results suggest that the developed UPLC method is precise, accurate and effective, and could be applied for quality control of HPL-4 formulation.

• Analytical Science and Technology
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• v.30 no.5
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• pp.295-302
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• 2017

This study presents a method validation for extraction and quantitative analysis of levulinic acid in soy sacues using high performance liquid chromatograph-photodiode array detector (HPLC-PDA). The levulinic acid in samples were extracted with distilled water, and then purified with C18 Sep-Pak cartridge. The calibration curves showed good linearity (R > 0.999) in a relatively wide concentration range ($2.5-400{\mu}g/mL$). Mean recoveries and relative standard deviation (RSD) of levulinic acid spiked in soy sauce samples at different spiking levels ($2.5-400{\mu}g/mL$; 6 point). Recoveries were 87.58-97.26 % with RSD less than 15 %, and limit of detection (LOD) and limit of quantification (LOQ) were 0.64 and $1.64{\mu}g/mL$, respectively. According to monitoring result with the established method, levulinic acid was found in 43 of 59 domestic commercial soy sauces, soy sauce based sauces and seasoned meats. The contamination levels were 0.44-1.23 mg/mL for soy sauces, 0.03-0.83 mg/mL for soy sauce based sauces and 8.43-38.94 mg/mL for seasoned meats. The results indicated to be rapidly and accurately qualifying levulinic acid and can be used as a suitable quality control method for soy sauce and soy sauce related commodities.

• Journal of the Korean Society of Food Science and Nutrition
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• v.43 no.11
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• pp.1791-1795
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• 2014

The objective of this study was to compare two extraction methods for determination of vitamin K1 (phylloquinone) in vegetables. In addition, analytical method validation parameters such as accuracy, precision, limit of detection (LOD), limit of quantification (LOQ), and linearity were calculated to ensure the method's validity. Vitamin K1 was quantified by reversed-phase HPLC using post-column derivatization and fluorescence detection ($Ex{\lambda}=243nm$, $Ex{\lambda}=430nm$). Higher analytical values were observed using solvent extraction compared to those from the enzyme extraction method. The results from the method validation showed high linearity in the calibration curve with a coefficient of correlation ($R^2$) of 0.9994. The LOD and LOQ were 0.1335 and 0.2784 ng/injection volume ($50{\mu}L$), respectively. The inter-day precision and inter-day precision were 2.0% and 2.1%, respectively. Overall recovery was close to 100% (n=5). The phylloquinone contents ranged from 9.42 to $1,212.57{\mu}g/100g$. Our study provides reliable data on the phylloquinone contents in commonly consumed vegetables in Korea.