• Journal of Food Hygiene and Safety
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• v.32 no.2
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• pp.89-95
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• 2017

A rapid, sensitive analytical method for glucuronolactone in beverages was developed and validated using hydrophilic interaction liquid chromatography coupled to electrospray ionization tandem mass spectrometry (HILIC-ESI-MS/MS). To determine the optimum analytical conditions for glucuronolactone, three different kinds of HILIC columns and two mobile phases with different pH values were examined. An amide-bonded stationary phase with a pH 9 acetonitrile-rich mobile phase was the best condition in terms of column retention, ESI-MS/MS response area, and signal-to-noise ratio. After extraction, glucuronolactone was separated through the HILIC amide column and detected by negative ESI-MS/MS in selected reaction monitoring (SRM) mode. Nine energy drinks sold in Korea were spiked with glucuronolactone at a concentration of 5 ng/mL; the Monster $Energy^{TM}$ sample showed the smallest peak area and its signal-to-noise ratio was used for method validation. Good linearity was obtained in the concentration range from 20 to 1500 ng/mL with a correlation coefficient > 0.998. The developed method had a limit of detection (LOD) of 6 ng/mL and a limit of quantitation (LOQ) of 20 ng/mL. The recovery of this method at concentration of 20, 100, 500, and 1000 ng/mL was 96.3%-99.2% with relative standard deviations (RSD) of 1.6%-14.0%. A reproducibility precision assessment at concentration of 100 and 500 ng/mL was carried out among three laboratories. The recovery of that evaluation was 95.1%-102.3% with RSD of 2.7%-7.0%. An analysis of variance indicated that there was no difference between the recovery results of the three laboratories at the 5% significance level. The validated method is applicable to inspecting beverages adulterated with glucuronolactone in Korea.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.49 no.3
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• pp.213-223
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• 2023

A total of 81 handmade soaps on sale on the market were collected from January to November 2022. To compare quality characteristics, all ingredients were referred to, and the pH, dry reduction, heavy metals (lead, arsenic, cadmium, antimony, and mercury), and contents of free alkali were measured. All soaps had a slightly alkaline pH of 7.9 to 11.2, average drying loss was 17.6%, and free alkali was hardly detected. The average values of all heavy metals were 0.104 ㎍/g for lead, 0.035 ㎍/g for arsenic, 0.002 ㎍/g for cadmium, 0.048 ㎍/g for antimony, and 0.0003 ㎍/g for mercury. The results of handmade soap were below the recommended in regulations on safety standards for cosmetics of Ministry of Food and Drug Safety.

• The Korean Journal of Pesticide Science
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• v.15 no.4
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• pp.357-365
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• 2011

Exposure measurement of agricultural worker to pesticide is one of important part of health risk assessment of pesticide. Therefore exposure matrices, apparatus, instruments and methods must be validated in advance to field experiment. In this study, method validation with an organophosphorus insecticide fenthion was carried out for exposure monitoring of agricultural worker. LOD and LOQ were 0.01 and 0.05 ng, respectively. Calibration curve linearity ($R^2$ > 0.999) and reproducibility (C.V. < 3%) were also excellent. Recovery at LOQ, 10LOQ and 100LOQ levels from gloves, socks, mask, patch, solid sorbent, glass fiber filter was 76~113% (C.V. < 3%). Trapping efficiency was 95~105% while no breakthrough was observed. Method validation for the exposure monitoring was established successfully through several experiments. Such method validation can be usually performed in laboratory and not much different for each pesticide so that, this techniques will be applied widely in research for pesticide exposure monitoring by combination with body surface area and respiration rates.

• Analytical Science and Technology
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• v.22 no.2
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• pp.128-135
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• 2009

This paper is the monitoring results of some heavy metals (lead, cadmium, arsenic, mercury) in herbal medicines and their intake rates. The monitoring of lead, cadmium, arsenic and mercury was carried out on 600 samples with 60 kinds of herbal medicines. And the transfer ratio of heavy metals in the water-boiled drinks w as calculated. The results show that lead was detected over the Maximum Residue Limits (MRL) in 10 samples (7 species). Cadmium was detected over the MRM in 69 samples (19 species). Arsenic was detected over the MRM in 3 samples (3 species). Mercury was detected over the MRM in 13 samples (10 species). We need continuously monitoring to ensure confidence and safety for these herbal medicines. In case of the water-boiled drink, average intake rates of lead, cadmium, arsenic and mercury are 9.77%, 6.72%, 26.1% and 6.79%, respectively.

• 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.

• Food Science of Animal Resources
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• v.38 no.1
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• pp.43-51
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• 2018

This study was conducted to analyze the microbiological contamination status of raw beef distributed in Korea, and evaluate the suitability of current aerobic plate count (APC) guidelines. We analyzed five years (2010-2014) of microbiological monitoring data obtained from the Ministry of Food and Drug Safety and investigated the microbiological status of raw beef collected from meat packing centers and meat shops in the Seoul/Gyeonggi, Gangwon, and Chungcheong regions in August 2015. From 2010-2014, most raw beef (>94%) displayed APC levels of < $1.0{\times}10^6CFU/g$. However, raw beef samples collected from all three regions in August 2015 had comparatively higher APC levels than those reported in previous years. To evaluate the relationship between the APC level and quality, changes in beef loin were evaluated during cold storage for 15 days at $4^{\circ}C$. On day 11, the mean APC level ($4.7{\times}10^6CFU/g$) conformed to current guidelines in Korea ($1.0{\times}10^7CFU/g$) and the pH value was 5.82. However, the sensory evaluation score for color and overall acceptability was under 3.0, meaning that the beef loin was not acceptable for eating. These results suggest that current APC guideline for raw beef should be lowered to $1.0{\times}10^6CFU/g$ to improve both the microbiological safety and palatability of raw beef.

• Journal of Environmental Health Sciences
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• v.43 no.4
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• pp.307-313
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• 2017

Objectives: Chemicals derived from various environment media contaminates food across the food supply chain. In Korea, levels of contaminants in food have been sporadically measured by monitoring programs of different government agencies. There is difficulty with data compilation and integrated analysis across media. Therefore, the aim of this study was to propose an overall integrated database and analytical platform design for the 'ECO-FOOD NET (Environmental COntaminant reduction platform for FOOD through an interagency collaboration NETwork)', a tool to support the reduction of environmental contaminants in food. Methods: We developed a new data structure and standardized protocols for the compilation of integrated data. In addition, we conducted subject-oriented logical and physical relational database modeling and created the architecture design of the platform. Results: We established a standardized code system related to exposure media and route, analysis method and food matrix. In addition, we designed the seven software modules of 'About the System', 'Introduction to Interagency Work', 'Media-Chemicals Profiles', 'Method Bank', 'Monitoring Data Base', 'Integrated Media Analysis', and 'Risk-Benefit Analysis'. Conclusions: This study will contribute to decision-making as a tool for executing risk management, such as sustainable reduction policies of contaminants in food.

• Tuberculosis and Respiratory Diseases
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• v.79 no.3
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• pp.158-164
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• 2016

Background: One to three percent of cases of acute tuberculosis (TB) require monitoring in the intensive care unit (ICU). The purpose of this study is to establish and determine the mortality rate and discuss the causes of high mortality in these cases, and to evaluate the clinical and laboratory findings of TB patients admitted to the pulmonary ICU. Methods: The data of patients admitted to the ICU of Yedikule Chest Diseases and Chest Surgery Education and Research Hospital due to active TB were retrospectively evaluated. Demographic characteristics, medical history, and clinical and laboratory findings were evaluated. Results: Thirty-five TB patients (27 males) with a median age of 47 years were included, of whom 20 died within 30 days (57%). The Acute Physiology and Chronic Health Evaluation II (APACHE II) and Sequential Organ Failure Assessment (SOFA) scores were significantly higher, and albumin and $PaO_2/FIO_2$ levels were significantly lower, and shock, multiple organ failure, the need for invasive mechanical ventilation and drug resistance were more common in the patients who died. The mortality risk was 7.58 times higher in the patients requiring invasive mechanical ventilation. The SOFA score alone was a significant risk factor affecting survival. Conclusion: The survival rate is low in cases of tuberculosis treated in an ICU. The predictors of mortality include the requirement of invasive mechanical ventilation and multiple organ failure. Another factor specific to TB patients is the presence of drug resistance, which should be taken seriously in countries where there is a high incidence of the disease. Finding new variables that can be established with new prospective studies may help to decrease the high mortality rate.

• Korean Journal of Clinical Pharmacy
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• v.26 no.1
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• pp.70-76
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• 2016

Background: The use of the extracts from evening primrose seeds as a health functional food has been gradually increased. Therefore, the monitoring and screening process has been considerably required for its quality control. Objective: This study aimed to estimate the measurement uncertainty associated with determination of penta-o-galloyl ${\beta}$-D-glucose (PGG) in extracts from evening primrose seeds by high-performance liquid chromatography. Methods: The sources of measurement uncertainty was expressed in accordance with mathematical/statistical theories of GUM & EURACHEM Guide. The expanded uncertainty was calculated by using the relative standard uncertainty between analytical result and sources of uncertainty in measurement (sample weight, final volume, extraction volume, standard solution, matrix and instrument etc). Results: In the results of 95% confidence interval, the uncertainty in measurement was $10,253.34{\pm}1,844.50{\mu}g/kg$ (k = 2.0). Conclusion: In this study, it showed that the value of uncertainty in measurement for determination of PGG in extracts from evening primrose seeds by HPLC has about 18.0% influence on PGG contents of the analytical results. The results would be very useful for the monitoring and screening of evening primrose seeds marketed in Korea for its quality control as dietary supplement.

• Korean Journal of Pharmacognosy
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• v.43 no.2
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• pp.137-146
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• 2012

Dipsaci Radix (Dipsacaceae) has been used as a tonic, an analgesic, anti-inflammatory and anti-complement agents in traditional herbal medicine for the therapy of low back pain, knee pain, rheumatic arthritis, traumatic hematoma, and bone fractures. A high-performance liquid chromatography-electrospray ionization-mass spectrometric method (HPLC-ESI-MS) was developed for the simultaneous quantitation method of the five compounds from the herbal drug: asperosaponin VI and asperosaponin XII (terpene glycosides), sweroside, loganin and dipsacus A(iridoid glycosides). HPLC separation of the analytes was achieved on a C18 column ($150{\times}2.0$ mm i.d., 5 ${\mu}m$) using the aqueous methanol containing 5 mM ammonium acetate with gradient flow of the mobile phase. Detection of the analytes was performed by positive ion electrospray ionization, and selected ion monitoring was used for data acquisition using m/z corresponding molecular adduct ion, $[M+NH_4]^+$ and $[M+H]^+$. Calibration graphs showed good linearity ($r^2$=0.9997) over the wide range of the analytes; intra- and inter-day precisions (RSD, %) were within 9.1% and the accuracy between 94.0-111.0%. Recoveries of the analytes through the assay procedure were in the range of 93.7-110.8%. Analytical results of the herbal drugs of Dipsaci Radix (17 samples) show wide distribution of the five marker compounds and clear difference of the species from Phlomidis Radix (4 samples). The developed method would provide a practical guide for the quality control of the herbal drug.