• Journal of Food Hygiene and Safety
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• v.25 no.3
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• pp.226-231
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• 2010

We aimed at the monitoring medroxyprogesterone acetate (MPA) residue amount in meats and confirmed the safety of its residue in meats. Optimized condition for analytical and instrumental methods was obtained by method validation. The limit of detection (LOD) and limit of quantification (LOQ) were validated at 1.5 and 5.0 ug/kg, respectively. The calibration curve showed good linearity ($r^2$ = 0.9968) within the concentration range of 5.0~50.0 ug/kg. We selected progesterone-d9 for internal standard, The recoveries in fortified meat ranged from 67.5 to 109.56% at the 3 spiking levels. As the regulation of MPA analysis method used by LC-MS/MS on other products have established. We selected 3 species of farm stock products (cattle, pig, chicken) and purchased at the markets of seven major cities. The total 196 of meat including 46 of domestic beef, 43 of import beef, 60 of domestic pork, 12 of import pork and 35 of domestic chicken. No residue of synthetic growth hormones were detected in cattle, pig and chicken samples tested.

• Journal of Food Hygiene and Safety
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• v.25 no.3
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• pp.203-208
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• 2010

In this study, the level of migration of 5 kinds of volatile organic compounds (VOCs) (toluene, styrene, ethylbenzene, isopropylbenzene and n-propylbenzene) into distilled water from polystyrene-made food containers was measured using Purge&Trap combined with GC/FID. The contents of the VOCs which have regulatory limits in Korea food code only for material specification were determined under three exposure conditions which were 30 min at $60^{\circ}C$, 30 min at $95^{\circ}C$ and actual situation of instant noodle intake. The calibration curve of 5 compounds showed good linearity ($^r2$ = 0.9976~0.9995) within the concentration range of 1~50 ng/mL. The limit of detection (LOD) and limit of quantification (LOQ) were validated at range of 0.041~0.092 and 0.135~0.304 ng/mL, respectively. The average migration contents of 5 compounds were below 5 ng/mL except for styrene. The average contents of styrene were highly detected at $95^{\circ}C$ for 30 min exposure (52.71 ng/mL). Under actual condition at instant noodle intake, the average contents of styrene was 17.23 ng/mL. The results demonstrated that the migration rate of VOCs was related to storage temperature and time.

• Food Science of Animal Resources
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• v.32 no.5
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• pp.571-577
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• 2012

This study was carried out to develop an analytical method for the determination of vitamin D in infant formula. Vitamin D was determined by column-switching high-performance liquid chromatography (HPLC) equipped with a reversed phase column and UV detector after saponification and extraction of the formula with an organic solvent. A preseparation column ($C_8$), focusing column ($C_{18}$), analytical column ($C_{18}$) and UV-Vis detector (254 nm) were used. The limits of detection (LOD) and the limits of quantification (LOQ) for vitamin D were estimated to be $1.51{\mu}g/kg$ and $4.95{\mu}g/kg$, respectively. The linearity, recovery, precision and accuracy of the analytical method for vitamin D were evaluated through the application of a SRM (Standard Reference Material) 1846 (National Institute of Standard & Technology, USA). The linearity of this method was calculated with a value of the coefficient of determination ($r^2$) ${\geq}0.9999$. The recovery of vitamin D was $85.20{\pm}3.00%$. The intra-assay precision for vitamin D was between $1.68{\pm}0.03%$ and $5.75{\pm}0.33%$, and the inter-assay precision for vitamin D ranged from $1.73{\pm}0.03%$ to $2.96{\pm}0.09%$. The intra-assay accuracy for vitamin D was between $100.03{\pm}2.77%$ and $102.01{\pm}0.59%$, and the inter-assay accuracy for vitamin D ranged from $99.00{\pm}1.53%$ to $102.01{\pm}3.04%$. The proposed method is optimal for the separation and quantification of vitamin D from infant formula.

• Food Science of Animal Resources
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• v.33 no.3
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• pp.417-424
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• 2013

A rapid and simple analytical method for the determination of 9 isomaltooligosaccharides (IMO) species in yoghurts was developed using dispersive solid phase extraction (dSPE) clean-up technic and high performance liquid chromatography with evaporative light-scattering detector (HPLC-ELSD). In this study, 9 IMO were extracted from samples simply with chemical reagent using ISO22662 IDF198 method and additional dSPE clean-up. The optimum instrument conditions for the determination were used carbohydrate ES $5{\mu}$ column with gradient elution of water and acetonitrile and ELS detector. The linearity of this method was expressed as the correlation coefficient ($r^2$), the results of IMO 9 species were shown in 0.9999. LOD and LOQ were respectively 7.9-22.1 mg/kg, 25.9-72.8 mg/kg. The accuracy of intra- and inter-day measurements were in the range from $84.3{\pm}4.5$ to $104.9{\pm}6.5%$, and the preceision of the intra- and inter-day measurements were in the range from 0.8 to 7.7%. The recoveries were from $84.3{\pm}4.5$ to $104.9{\pm}6.5%$. The determination results of IMO 9 species for the 9 yoghurts circulated in the market were in the range from $0.317{\pm}0.007$ to $1.624{\pm}0.050$ g/100 g. The newly developed method is appropriate for the determination of IMO in yoghurts, is a rapid and simple method with excellent resolution in compared with previous method.

• Korean Journal of Environmental Agriculture
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• v.39 no.3
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• pp.246-252
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• 2020

BACKGROUND: Pesticides are broadly used to control weeds and pests, and the residues remaining in crops are managed in accordance with the MRLs (maximum residue limits). Therefore, an analytical method is required to quantify the residues, and we conducted a series of analyses to select and validate the quick and simple analytical method for tolpyralate in five agricultural products using QuEChERS (quick, easy, cheap, effective, rugged and safe) method and LC-MS/MS (liquid chromatography-tandem mass spectrometry). METHODS AND RESULTS: The agricultural samples were extracted with acetonitrile followed by addition of anhydrous magnesium sulfate, sodium chloride, disodium hydrogencitrate sesquihydrate and trisodium citrate dihydrate. After shaking and centrifugation, purification was performed with d-SPE (dispersive-solid phase extraction) sorbents. To validate the optimized method, its selectivity, linearity, LOD (limit of detection), LOQ (limit of quantitation), accuracy, repeatability, and reproducibility from the inter-laboratory analyses were considered. LOQ of the analytical method was 0.01 mg/kg at five agricultural products and the linearity of matrix-matched calibration were good at seven concentration levels, from 0.0025 to 0.25 mg/L (R²≥0.9980). Mean recoveries at three spiking levels (n=5) were in the range of 85.2~112.4% with associated relative standard deviation values less than 6.2%, and the coefficient of variation between the two laboratories was also below 13%. All optimized results were validated according to the criteria ranges requested in the Codex Alimentarius Commission (CAC) and Ministry of Food and Drug Safety (MFDS) guidelines. CONCLUSION: In conclusion, we suggest that the selected and validated method could serve as a basic data for detecting tolpyralate residue in imported and domestic agricultural products.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.24 no.3
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• pp.345-352
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• 2014

Objectives: This study is aimed to describe the current situation about urinary biomarker N-methylformamide(NMF) for workers exposed to N,N-dimethylformamide(DMF) according to industrial classification. Materials: Special health examination records of the workers who had undergone urinary biological monitoring in 2013 were collected. The numbers and percentage of workers, whose urinary NMF values were above the limit of detection(LOD) and above the biological exposure index(BEI) were calculated. Health relatedness with DMF as judged by their doctors was also described. All description was classified according to the $9^{th}$ Korean Standard Industrial Classification(KSIC). Results: It appeared that most workers exposed to DMF belong to manufacturing section(80.7%). The geometric mean(GM) values of urinary NMF were 6.25 mg/L, 3.54, and 3.86 for the manufacturing section, professional, scientific and technical activities section, and for the construction section respectively. In detail, it seemed that division of textiles(except apparel) (GM 7.51 mg/L), division of leather, luggage and footwear(11.59 mg/L), and division of rubber and plastic products(6.89 mg/L) were highly exposed to DMF with a high percentage of workers with urinary NMF values above BEI. This was probably due to the effect of skin absorption that the division of leather, luggage and footwear showed the highest urine NMF GM. Conclusions: It seemed that workers in manufacture industries such as textile, leather, luggage, footwear, rubber and plastic products were highly exposed to DMF. So, efforts should be focused on those industries in order to effectively diminish worker's exposure. Further studies to compare DMF air-monitoring with bio-monitoring according to industrial classification should be considered.

• Journal of Food Hygiene and Safety
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• v.22 no.2
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• pp.88-92
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• 2007

Isopropylthioxanthone(ITX) is used as a photoinitiator In UV-cured inks, triggering the radical polymerization of the acrylic component of such inks and thus causing the liquid ink film to cure. Recently ITX was detected in carton packed food in Italy. In order to cope with risk issues of overseas and acquire monitoring data on ITX, we have established the method using HPLC/FLD for ITX analysis after reviewing parameters of the analytical methods. Limit of detection (LOD) and limit of quantification (LOQ) were 0.02 ppb and 0.1 ppb, and linearity and RSD (%) were 0.9991 and 1.09, respectively. We have investigated ITX levels migrated to food on 87 commercial products packed in carton and ITX was not detected any food. Therefore it is supposed that UV-cured ink containing ITX as photoinitiator is not currently used in printing of carton pack in Korea.

• Journal of Food Hygiene and Safety
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• v.32 no.5
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• pp.404-410
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• 2017

An analytical method for determination of propylene glycol alginate (PGA) in food products was developed by HPLC-size-exclusion chromatography. The GF-7M HQ column and LT-ELSD detector were determined by considering the instrumental analysis conditions for PGA analysis. The pretreatment method for the analysis of PGA was suitable for 3 hr extraction at $20^{\circ}C$ and 150 rpm according to the extraction temperature. Linearity ($R^2$) for the analysis of PGA was 0.9873 at calibration curve range of 300, 500, 700, 1,000, and 1,500 mg/kg (5 points). The limit of detection and limit of quantification of PGA on HPLC system was 171.43 and 519.50 mg/kg, respectively. The accuracy and coefficient of variation obtained by size-exclusion chromatography were 86.1~110.4% and 4.1~13.5%, respectively. By applying the HPLC-size-exclusion chromatography system, it was possible to analyze the contents of PGA in 134 different types of food products.

• Journal of Food Hygiene and Safety
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• v.32 no.5
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• pp.343-347
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• 2017

The analytical method of silicon dioxide ($SiO_2$) in health functional food products was developed employing inductively coupled plasma optical emission spectrometry (ICP-OES) method assisted by acid (hydrofluoric acid and boric acid) digestion in open system without alkali fusion. The limit of detection (LOD) and limit of quantification (LOQ) of this method were found to be 0.07 and 0.20 mg/L, respectively. Linearity ($r^2$) and linear range were 0.99 and 0.20~20.0 mg/L, respectively. The accuracy and precision of $SiO_2$ (0.4, 1.0, and 2.0%, w/w) in spiked glucosamine exhibited to be the range of 90.22~94.14% and 0.72~1.67%, respectively. The contents of $SiO_2$ in 11 health functional food products were detected in range of 0.02~1.80% (w/w). Every sample showed below content of the permitted use level (2%, w/w) of $SiO_2$. Therefore ICP-OES method with acid can analyze the content of $SiO_2$ in health functional food products easily and rapidly. Consequently, the application of specification analysis of $SiO_2$ in health functional food products could be a significant work.

• Korean Journal of Food Science and Technology
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• v.39 no.6
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• pp.715-720
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• 2007

The levels of butyltin compounds in poly(vinyl chloride) (PVC) food packaging using gas chromatography/mass spectrometry (GC/MS) were monitored. The analytical method, involving the ethylation with sodium tetraethylborate, was found to be selective and sensitive for mono-n-butyltin (MBT), di-n-butyltin (DBT), and tri-n-butyltin (TBT), validated by a $0.005\;{\mu}g/mL$ limit of detection (LOD), an $R^2>0.999$ for linearity, and >90% of recovery, respectively. Finally, none of the commercial food wraps and gaskets showed detectable levels of butyltin compounds.