• Journal of Food Hygiene and Safety
• /
• v.35 no.3
• /
• pp.225-233
• /
• 2020

By the standards and specifications for hygiene products, three test methods for formaldehyde are specified for each item type of hygiene product. After derivatization using acetylacetone and 2,4-dinitrophenylhydrazine (2,4-DNPH), formaldehyde is analyzed by spectrophotometer and high-performance liquid chromatography (HPLC). Validation of the three test methods was performed on tissue, diaper lining and waterproof layer, and panty liner products. The results of linearity (R²), limit of detection (LOD), limit of quantification (LOQ), recovery rate (%) and reproducibility (%), showed that all three methods are suitable for analyzing formaldehyde in hygiene products. After derivatization with 2,4-DNPH and cetylacetone, formaldehyde was analyzed at 0, 3, 6, 9, 24 and 48 hours by HPLC. Formaldehyde derivatized with 2,4-DNPH showed no statistically significant change in formaldehyde peak area over time (P>0.05). But, acetylacetone-derivatizated formaldehyde showed a negative correlation coefficient (r) over time (P<0.01). We investigated the residual amounts of formaldehyde in 205 hygiene products distributed in Busan. Among 74 disposable diaper products tested, 73 had low concentrations of formaldehyde (0.13-29.87 mg/kg). Moreover, formaldehyde was not detected in any of 78 tissue, 27 disposable paper towel, 12 disposable dishcloth, 7 paper cup, one brand of paper straw and 6 disposable napkin products.

• Korean Journal of Food Science and Technology
• /
• v.38 no.6
• /
• pp.730-737
• /
• 2006

High performance liquid chromatographic methods for the simultaneous determination of 12 biogenic amines were developed and contents of biogenic amines in 23 varieties of Korean commercial fermented food were analyzed. Dansyl derivatives of biogenic amine were very stable and had good peak resolution. Except agmatine, the recovery of biogenic amines from soybean paste with extraction of 0.1 N HC1 added biogenic amines to soybean paste was greater 85%. The calibration curve showed good linearity over a concentration range up to 50 ${\mu}g/mL$. In the determination of biogenic amine level in Korean commercial fermented foods, doenjang and chungkukjang (fermented soybean pastes), soy sauce, anchovy and pacific sand lance liquid jeotkal (fermented fish sauce products), and cabbage kimchi had high level biogenic amines. Especially, traditional doenjang had a histamine (HIS) level of 952.0 mg/kg, a tyramine (TYR) level of 1,430.7 mg/kg. Most cheese had low level of biogenic amines, but one Gouda cheese had a tyramine (TYR) level of 97.5 mg/kg. A low level of biogenic amines was detected in wines, beer, yoghurt, and sausage. Putrescine (PUT), cadaverine (CAD), tryptamine (TRY), histamine (HIS), tyramine (TYR), and 2-phenylethylamine (PHE) were mainly formed in fermented foods by the action of microorganism, so their levels were high with a range. On the other hand, spermidine (SPD), spermine(SPM), serotonin (SER), noradrenaline (NOR), and dopamine (DOP) were formed originally via biosynthesis with consequent low level.

• Asian Pacific Journal of Cancer Prevention
• /
• v.14 no.12
• /
• pp.7509-7515
• /
• 2013

To assess the risk of cancers associated with sleep duration using meta-analysis of published cohort studies, we performed a comprehensive search using PubMed, Embase and Web of Science through October 2013. We combined hazard ratios (HRs) from individual studies using meta-analysis approaches. A random effect dose-response analysis was used to evaluate the relationship between sleep duration and cancer risk. Subgroup analyses and sensitivity analyses were also performed. Publication bias was evaluated using Funnel plots and Begg's test. A total of 13 cohorts from 12 studies were included in this meta-analysis, which included 723, 337 participants with 15, 156 reported cancer outcomes during a follow-up period ranging from 7.5 to 22 years. The pooled adjusted HRs were 1.06 (95% CI: 0.92, 1.23; P for heterogeneity =0.003) for short sleep duration, 0.91 (95% CI: 0.78, 1.07; P for heterogeneity <0.0001) for long sleep duration. In subgroup analyses stratified by cancer type, long duration of sleep showed an inverse relation with hormone-related cancer (HR=0.79; 95% CI: 0.65, 0.97; P for heterogeneity =0.009) and a greater risk of colorectal cancer (HR=1.29; 95% CI: 1.09, 1.52; P for heterogeneity =0.346). Further meta-analysis on dose-response relationships showed that the relative risks of cancer were 1.00 (95% CI: 0.99, 1.01; P for linear trend=0.9151) for one hour of sleep increment per day, and 1.00 (95% CI: 0.98, 1.01; P for linear trend=0.7749) for one hour of sleep increment per night. No significant dose-response relationship between sleep duration and cancer was found on non-linearity testing (P=0.5053). Our meta-analysis suggests a positive association between long sleep duration and colorectal cancer, and an inverse association with incidence of hormone related cancers like those in the breast. Studies with larger sample size, longer follow-up times, more cancer types and detailed measure of sleep duration are warranted to confirm these results.

• Korean Journal of Food Science and Technology
• /
• v.39 no.4
• /
• pp.372-379
• /
• 2007

A high-performance liquid chromatography-electrospray ionization (HPLC-ESI) tandem MS was developed for the rapid and simultaneous determination of forbidden medicines in dietary supplements. Thirteen medicinal components such as PDE-5 inhibitors and their analogues, and the newly identified dimethylsildenafil and xanthoanthrafil, were included in this study. After tentative standardization of molecular ions in both polarities using thirteen references on the mass spectrometer, with ESI-continuous infusion via the syringe pump method, the relative intensity of the ions present in the resulting spectra was quantitatively compared. From the results, the ion mode was selected depending on each reference's characteristics. A HPLC method coupled with the ESI mode was developed considering the matrix effect and interference depending on the type of sample. The validation test of the developed method was followed by carrying out precision, accuracy, recovery, sensitivity and linearity, etc. The method showed sufficiently high sensitivity, reproducibility, and specificity, and produced 4 times faster results when compared with the existing HPLC/UV method for the determination of forbidden compounds in dietary supplements.

• Analytical Science and Technology
• /
• v.28 no.6
• /
• pp.385-397
• /
• 2015

Harmful and potentially harmful constituents (HPHCs) are chemical compounds in tobacco smoke that cause harm to smokers and non-smokers. This study established and validated methods for the analysis of HPHCs from mainstream cigarette smoke. The analyzed HPHCs were categorized into seven groups: aromatic amines, volatile organic compounds (VOCs), heavy metals, tobacco specific nitrosamines (TSNAs), benzo[a]pyrene (B[a]P), ammonia, and carbonyl compounds. The methods were validated by specificity, linearity, limit of detection (LOD), accuracy, precision, and recovery. These validated methods were then applied to the reference cigarettes (1R5F, 3R4F). The correlation coefficients (r²) for the calibration curves of the seven groups were over 0.995. The LODs showed values of 0.01-0.04 ng/cig cig for aromatic amines, 0.01-0.16 μg/cig for VOCs, 0.01-1.27 ng/cig for heavy metals, 0.06-0.28 ng/cig for TSNAs, 0.04 ng/cig for benzo[a]pyrene, 0.08 μg/cig for ammonia, and 0.78-1.77 μg/cig for carbonyl compounds. The precisions obtained from the intra and inter-day batches were less than 15%. The accuracy and the recovery range were less than 15% and 79.2-117.5%, respectively. The proposed methods can therefore be applied for determining HPHCs in tobacco mainstream smoke.

• The Korean Journal of Pesticide Science
• /
• v.19 no.3
• /
• pp.161-173
• /
• 2015

The multiresidue method 4.1.2.2 in Korea Food Code was extended for the analysis of 24 unregistered pesticide residues. The method includes acetonitrile extraction, liquid-liquid partition, Florisil SPE clean-up and GC analysis. The limits of quantification (LOQ) range of the method was 0.02~0.05 mg/kg for orange, brown rice and banana. The linearity for targeted pesticides were $R^2$ > 0.99 at the level ranged from 0.05 to 5 mg/L. Recovery test was performed at two concentration levels of LOQ and 4~10 times of LOQ. Recoveries and relative standard deviations (RSDs) of target pesticides were acceptable, showing 70~120% range and less than 20%, respectively, except for ethiprole, picloram and sulcotrion. This method is effectively applicable to routine analysis of target pesticides in orange, brown rice and banana.

• Journal of Food Hygiene and Safety
• /
• v.35 no.1
• /
• pp.23-30
• /
• 2020

This study investigated the migration levels of lead (Pb), cadmium (Cd), and arsenic (As) from food contact articles (glassware, ceramics, enamelware, and earthenware) into a food stimulant (4% v/v, acetic acid). Migration tests were performed at 25℃ for 24 h and all analyses were performed using Inductively-Coupled Plasma Mass Spectrometry (ICP-MS). The method was validated by linearity of calibration curves, limit of detection (LOD), limit of quantification (LOQ), recovery, precision, and uncertainty. In glassware, the migration concentrations ranged from not-detected (N.D.) to 752.21 ㎍/L and N.D. to 1.99 ㎍/L for Pb and Cd, respectively. In ceramics, the migration concentrations ranged from N.D. to 1,955.86 ㎍/L, N.D. to 74.06 ㎍/L, and N.D. to 302.40 ㎍/L for Pb, Cd, and As, respectively. In enamelware, the migration concentrations ranged from N.D. to 4.48 ㎍/L, N.D. to 7.00 ㎍/L, and N.D. to 52.00 ㎍/L for Pb, Cd, and Sb, respectively. In earthenware, the migration concentrations ranged from N.D. to 13.68 ㎍/L, N.D. to 0.04 ㎍/L, and N.D. to 6.71 ㎍/L for Pb, Cd, and As, respectively. All results were below the migration limits of Korea standards and specifications for food utensils, containers, and packages.

• Journal of Food Hygiene and Safety
• /
• v.39 no.2
• /
• pp.72-82
• /
• 2024

This study aimed to develop a scientifically and systematically standardized xylooligosaccharide analytical method that can be applied to products with various formulations. The analysis method was conducted using HPLC with Cadenza C₁₈ column, involving pre-column derivatization with 1-phenyl-3-methyl-5-pyrazoline (PMP) and UV detection at 254 nm. The xylooligosaccharide content was analyzed by converting xylooligosaccharide into xylose through acid hydrolysis. The pre-treated methods were compared and evaluated by varying sonication time, acid hydrolysis time, and concentration. Optimal equipment conditions were achieved with a mobile phase consisting of 20 mM potassium phosphate buffer (pH 6)-acetonitrile (78:22, v/v) through isocratic elution at a flow rate of 0.5 mL/min (254 nm). Furthermore, we validated the advanced standardized analysis method to support the suitability of the proposed analytical procedure such as specificity, linearity, detection limits (LOD), quantitative limits (LOQ), accuracy, and precision. The standardized analysis method is now in use for monitoring relevant health-functional food products available in the market. Our results have demonstrated that the standardized analysis method is expected to enhance the reliability of quality control for healthy functional foods containing xylooligosaccharide.

• Journal of Pharmaceutical Investigation
• /
• v.38 no.4
• /
• pp.261-267
• /
• 2008

The aim of the present study was to evaluate the bioequivalence of two gabapentin preparations. We used Neurontin tablet 800 mg (Pfizer Korea Inc.) as a reference drug for bioequivalence of Gabalep tablet 800 mg (Chong Kun Dang Pharmaceutical Co., Korea), and performed this whole study according to the guidelines of Korea Food and Drug Administration (KFDA). Twenty five healthy male volunteers were administered with each drug in a randomized $2{\times}2$ cross-over study with one week washout interval. After drug administration, blood was taken at predetermined time intervals ($0{\sim}24$ hours) and the concentrations of gabapentin in serum were determined using an high performance liquid chromatography-tandem mass spectrometer (LC-MS/MS) employing electrospray ionization technique and operating in multiple reaction mornitoring (MRM). The analytical method was validated in specificity, accuracy, precision and linearity. The phar-macokinetic parameters such as AUCt and Cmax were calculated and ANOVA test was utilized for the statistical analysis of the parameters using logarithmically transformed AUCt and Cmax. $Mean{\pm}SD$. of AUCt and Cmax value for reference drug and test drug were $29.94{\pm}9.23\;({\mu}g/mL{\cdot}hr)$ and $3.12{\pm}1.11\;({\mu}g/mL{\cdot}hr)$, and $31.48{\pm}9.77\;({\mu}g/mL{\cdot}hr)$ and $3.15{\pm}1.03\;({\mu}g/mL)$, respectively. The 90% confidence intervals using logarithmically transformed data were within the acceptance range of log(0.8) to log(1.25) for AUCt and Cmax, respectively. These results indicate that Gabalep tablet 800 mg is bioequivalent to Neurontin tablet 800 mg.

• Journal of Food Hygiene and Safety
• /
• v.28 no.1
• /
• pp.45-49
• /
• 2013

This study aimed to determine heavy metal contents in sesame oil samples produced in Korea through microwave-assisted acid digestion without using an emulsifier. Three heavy metal, cadmium (Cd), lead (Pb) and arsenic (As) in twelve sesame oil samples were determined by ICP-MS. The validation of analysis method was checked by standard addition method (10 and $100{\mu}g/kg$). As a result, linearity ($R^2$) was above 0.999 and RSDs were lower than 4%. The recovery of Cd, Pb and As ranged between 98.5-101.6%, 100.3-101.3%, and 102.1-111.2%, respectively. The detected ranges in sesame oil samples were as follows; N.D. to $0.109{\mu}g/g$ for Cd, 0.014 to $0.200{\mu}g/g$ for Pb and 0.014 to $0.125{\mu}g/g$ for As, respectively. Therefore, sesame seeds and products grown in heavy metal-polluted regions which are used as food should be given priority attention and consideration.