• Journal of Food Hygiene and Safety
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• v.34 no.3
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• pp.263-268
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• 2019

Methanol is a toxic alcohol used in various products such as antifreeze, detergent, disinfectant and industrial solvent. In the human body, methanol is oxidized to formaldehyde and formic acid, which can lead to metabolic acidosis, optic nerve impairment, and death. In this study, the methanol levels in detergents (n=191) and rinse aids (n=13) were analyzed by gas chromatography-headspace-mass spectrometry (GC-HS-MS). Limit of detection was 1.09 mg/kg, accuracy and precision were 91.1-97.9% and <10%, and it was suitable for quantitative analysis. This analysis method was simple and fast with a higher recovery rate than the conventional MFDS (Ministry of Food and Drug Safety) method of diluting the sample in water and putting it in a headspace vial.

• Analytical Science and Technology
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• v.32 no.2
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• pp.35-47
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• 2019

In this study, high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was employed to detect 26 antidiabetic compounds in adulterated dietary supplements using a simple, selective method. The work presented herein may help prevent incidents related to food adulteration and restrict the illegal food market. The best separation was obtained on a Shiseido Capcell Pak(R) C18 MG-II ($2.0mm{\times}100mm$, $3{\mu}m$), which improved the peak shape and MS detection sensitivity of the target compounds. A gradient elution system composed of 0.1 % (v/v) formic acid in distilled water and methanol at a flow rate of 0.3 mL/min for 18 min was utilized. A triple quadrupole mass spectrometer with an electrospray ionization source operated in the positive or negative mode was employed as the detector. The developed method was validated as follows: specificity was confirmed in the multiple reaction monitoring mode using the precursor and product ion pairs. For solid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL, and for liquid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL. Satisfactory linearity was obtained from calibration curves, with $R^2$ > 0.99. Both intra and inter-day precision were less than 13.19 %. Accuracies ranged from 80.69 to 118.81 % (intra/inter-day), with a stability of less than 14.88 %. Mean recovery was found to be 80.6-119.0 % and less than 13.4 % RSD. Using the validated method, glibenclamide and pioglitazone were simultaneously determined in one capsule at concentrations of 1.52 and 0.53 mg (per capsule), respectively.

• Journal of the Korean Chemical Society
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• v.65 no.6
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• pp.433-440
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• 2021

Surfactants are organic compounds that have both hydrophilic and non-polar parts in one molecule, classified as non-ion, anion, cation, and amphoteric surfactants according to the charge of hydrophilic parts in aqueous state. A trace amounts may remain when vegetables and fruits are washed using type1 detergent (Vegetable and fruit detergent), and there is a possibility of exposure to the human body through ingestion. This study developed the simultaneous analysis method for 5 surfactants with LC-MS/MS for analysis of detergent residues after washing vegetables and fruits with detergent. The mobile phase used distilled water and acetonitrile containing 50 mM ammonium formate and 0.1% formic acid and was analyzed using a gradient method using XBridge BEH C8 column. The accuracy of the established method was 83.9-112.1%, and the precision was less than 20%. The detection limit was 7.0 (SLS) to 29.0 (SLES-N3) ㎍/L, and the correlation coefficient (r²) of calibration line regression was greater than 0.99, it is considered suitable for the analysis of trace amounts of surfactant components remaining in vegetables and fruits.

• Korean Journal of Environmental Agriculture
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• v.42 no.3
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• pp.203-210
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• 2023

Ferimzone Z is a fungicide for effectively controlling rice blast. Under light irradiation conditions, it undergoes a rapid conversion to its E-stereoisomer. Given the importance of isomers in risk assessments of residues in crops, an analytical method was developed for individual isomer quantification. A comparative analysis performed using two columns in HPLC-MS/MS demonstrated that the isomers were successfully separated using the Cadenza column. For the brown rice sample preparation, 5 g of the homogenized sample was saturated with 7 mL of water. The sample was then extracted with a 10 mL mixed solvent of acetonitrile and ethyl acetate (1:1, v/v) that contained 0.1% formic acid, and it was subsequently partitioned with magnesium sulfate and sodium chloride. The upper layer was purified using dSPE containing C₁₈ and PSA sorbents. The established method was subjected to method validation, and it showed recovery rates of 90.6-98.8% (RSD ≤ 3.9%) at concentrations of 0.01, 0.1, 2 mg/kg, with a soft matrix effect (%ME) ranging from -3.1% to +6.5%. This method can be employed in monitoring studies of brown rice to determine the conversion ratio from the Z isomers to the E isomers.

• Korean Journal of Environmental Agriculture
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• v.42 no.1
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• pp.71-81
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• 2023

An accurate and easy-to-use analytical method for determining isocycloseram and its metabolites (SYN549431 and SYN548569) residue is necessary in various food matrixes. Additionally, this method should satisfy domestic and international guidelines (Ministry of Food and Drug Safety and Codex Alimentarius Commission CAC/GL 40). Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) was used to determine the isocycloseram and its metabolites residue in foods. To determine the residue and its metabolites, a sample was extracted with 20 mL of 0.1% formic acid in acetonitrile, 4 g magnesium sulfate anhydrous and 1 g sodium chloride and centrifuged (4,700 G, 10 min, 4℃). To remove the interferences and moisture, d-SPE cartridge was performed before LC-MS/MS analysis with C₁₈ column. To verify the method, a total of five agricultural commodities (hulled rice, potato, soybean, mandarin, and red pepper) were used as a representative group. The matrix-matched calibration curves were confirmed with coefficients of determination (R²) ≥ 0.99 at a calibration range of 0.001-0.05 mg/kg. The limits of detection and quantification were 0.003 and 0.01 mg/kg, respectively. Mean average recoveries were 71.5-109.8% and precision was less than 10% for all five samples. In addition, inter-laboratory validation testing revealed that average recovery was 75.4-107.0% and the coefficient of variation (CV) was below 19.4%. The method is suitable for MFDS, CODEX, and EU guideline for residue analysis. Thus, this method can be useful for determining the residue in various food matrixes in routine analysis.

• Korean Journal of Environmental Agriculture
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• v.42 no.2
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• pp.139-151
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• 2023

Sulfonylurea herbicides are widely used in agriculture because they have a long residual period and high selectivity. An analytical method was developed using QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) technique for simultaneous determination of sulfonylurea herbicide residues in agricultural products by liquid chromatography tandem mass spectrometry and for establishment MRL (Maximum Residue Limit) of those herbicides in Korea. Extraction was performed using acetonitrile containing 0.1% formic acid with MgSO₄ (anhydrous magnesium sulfate) and NaCl (sodium chloride) and the extract was cleaned up using MgSO₄ and C₁₈ (octadecyl). The matrix-matched calibration curves were composed of 7 concentration levels from 0.001 to 0.25 mg/kg and their coefficients of determination (R²) exceeded 0.99. The recoveries of three spiking levels (LOQ, 10LOQ, 50LOQ, n=5) were in the range of 71.7-114.9% with relative standard deviations of less than 20.0% for all the five agriculture products. All validation values met criteria of the European Union SANTE/11312/2021 guidelines and Food and Drug Safety Evaluation guidelines. Therefore, the proposed analytical method was accurate, effective, and sensitive for sulfonylurea herbicide residues determination in agricultural commodities.

• Journal of Practical Agriculture & Fisheries Research
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• v.25 no.4
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• pp.53-59
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• 2024

The purpose of the study was to examine the effects of initial body weight and synbiotics supplementation in the diet on growth performance of weaned pigs. A total of 80 crossbred pigs (Landrace×Yorkshire×Duroc, d 28±3, body weight 6.40±1.70 kg) were randomly distributed 4 treatments (4 replication, 5 pigs/replication). The treatments were 1) high initial body weight group (PC), 2) low initional body weight group (NC), 3) low initial body weight with 0.2% antibiotics (amoxicillin) supplementaion group (AB), 4) low initial body weight with 0.2% synbiotics (AllTech^® Bio-Mos 0.3%, 0.3%, Bacillus subtillis 0.1%, formic acid 0.1%) supplementation group (Syn). AllTech^® Bio-Mos is consist of at least 25% of glucomannanprotein extracted from the cell wall of Saccaromycess cerevisae. Growth performance was measured during 28 d. Average daily gain (ADG) of AB and Syn groups were significantly (p<0.05) higher than that of NC group. However, final body weight at the end of experiment were not different among NC, AB, and Syn groups. Initial body weight and final body weight of PC group were statistically (p<0.001) higher compared to those of other groups. Additionally, PC showed the tendency of lower average daily feed intake and higher ADG, thereby lower feed conversion ratio compared with other groups. Therefore, the current results imply that supplementation of antibiotics and synbiotics in diets for weaned pigs could not catch up with significant differences in initial body weight.

• Journal of The Korean Society of Grassland and Forage Science
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• v.17 no.2
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• pp.187-198
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• 1997

This experiment was conducted to evaluate effects of wilting and additives on fermetation characteristics, quality and aerobic stability of silage of rye(Seca1e cereale L.) harvested at the early heading stage. Harvested rye was wilted or mixed with beet pulp and then treated with formic acid or lactic acid bacteria(LAB) inoculant. Treatments were consisted of direct cut(DC), wilted(WT), beet pulp added(BP), direct cut and formate applied(DF), wilted and formate applied(WF), beet pulp and formate applied(BF), direct cut and LAB inoculated(DL), beet pulp added and LAB inoculated(BL), and wilted and LAB inoculated(WL) silages. Afler 70 days of ensiling period, the silages were opened and exposed to air for 7 days, and the silages of opening day(0 day) were compared with the silages exposed to air for 7 days(7 day). 1. LAB inoculated rye silages(DL, WL, BL) lowered pH values effectively eom the third day of ensiling and showed most stable pattern of pH changes during the initial fermentation process. Direct cut and formate applied(DF), beet pulp and formate applied(BF) and beet pulp added(BP) silages were also effective in lowering pH from the seventh day thai direct cut treatment(DC). 2. pH was low below 3.7 in all treatments of 0 day. After 7-day period of aerobic exposure, DL and WL showed considerable increases in pH from 3.5 and 3.4 to 8.3 and 6.4, respectively. 3. Direct cut rye silages(DF, DC, DL) and beet pulp and formate treatment(BF) produced effluent of 121.2, 85.9, 80.3 and 34.2 mlkg, respectively and these were greater than others(P<0.01). Beet pulp retained 1.61 I/kg of effluent at the application rate of 50 kg/t in comparing BP with DC, and formate application increased the amount of effluent in comparing DF and BF with DC and BP, respectively(P<0.01). 4. Beet pulp and LAB treatment(B1) was highest in content of lactate as 3.1% and formate treated silages(DF, WF, BF) showed lower content of lactate and total acid than others. LAB inoculated(D1, WL, BL) and wilted (WT) silages were graded to be good quality as a second group by the Flieg's score. Formate applied silages (DF, WF, BF) were graded as a foum group lower than DC by one. 5. Residual content of WSC of rye silage was higher in BP, BF, DL and BL than direct cut treatment(M3) (P< 0.01). Formate application had a tendency to increase the content of residual content of WSC. 6. For the ratio of NH3-N to Total N, wilted and LAB inoculated(W1) and direct cut and LAB inoculated(D1) silages were lowest on 0 day as 8.9 and 9.3% respectively. But after 7-day period of aerobic exposure, WL and DL showed largest increase of the ratio of $NH_3-N$ to Total N from 0 day(P<0.01). 7. On 0 day wilted(WT), beet pulp and formate treatment(BF), and beet pulp and LAB treatment(B1) were lower than direct cut treatment(DC) for NDF and ADF concentrations consistently. Formate applied silages (DF, WF, BF) made little change in ADF and NDF concentrations during 7 day period of aerobic exposure. DL and WL showed a large increase in ADF and NDF concentrations under aerobic condition(P<0.01). 8. IVDMD values of wilted(WT), beet pulp added(BP), wilted and LAB inoculated(W1) and beet pulp added and LAB inoculated(B1) silages were higher than direct-cut treatmentPC) as 84.7, 84.7, 84.4 and 83.0%, respectively on 0 day. But during 7-day period of aerobic exposure, a great decreae in IVDMD of WL was showed(P<0.01). The experimental results indicate that wilted silage(WT) could be recommended as the most effective treatment for reducing efluent and increasing quality and feed value of rye silage without deteriorating aerobic stability more than direct cut treatment(DC). Additionally, under unfavorable weather condition beet pulp added and LAB inoculated treatment(T3L) might be the possible alternative for successful ensiling of forage rye.

• Restorative Dentistry and Endodontics
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• v.24 no.1
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• pp.100-115
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• 1999

The purpose of this study was to investigate the distribution of calcitonin gene-related peptide containing nerve fibers in rat pulp after dentinl injury by means of immunohistochemistry and confocal laser scanning microscope. The Spague-Dawley rats weighing about 250-300gm were used. The animals were devided into normal control and experimental groups. Experimental animals were sacrified 1, 2, 4, 7, 10, 21days after dentinal injury (dentin cutting, and then acid etching with 35% phosphoric acid) on the maxillary molar teeth. The maxillary teeth and alveolar bone were removed and immersed in the 4% paraformaldehyde in 0.1M phosphate buffer (pH 7.4), then were decalcified with 15% formic acid for 10 days. Serial frozen $50{\mu}m$ thick sections were cut on a cryostat. The rabbit CGRP antibody was used as a primary antibody with a dilution of 1:2000 in 0.01M PB. The sections were incubated for 48 hours at $4^{\circ}C$, and placed into biotinylated antirabbit Ig G as a secondary anti body with dilution of 1:200 in 0.01M PB and incubated in ABC(avidin-biotin complex). The peroxidase reaction was visualized by incubating the sections in 0.05% 3,3 diaminobenzidine tetrahydrochloride containing 0.02% $H_2O_2$. For the confocal laser scanning microscopic examination, Primary antibody reaction was same as immunoperoxidase stainning, but fluorescein isothiocyanate(FITC)-conjugate antirabbit IgG as a secondary antibody was used. The confocal laser scanning microscope was used for the examination. A series of images of optical sections was collected with a 20x objective at $3{\mu}m$ intervals throughout the depth of specimen. FITC fluerescence was registrated through a 488nm and 568nm excitation filter, and images were saved on optical disk. The stereoscopic images and three dimentionnal images were reconstructed by computer software, and then were analyzed. The results were as follows : 1. In normal control group, CGRP containing nerve fibers were coursed through the root with very little branching, and then formed a dense network of terminals in coronal pulp. 2. A slight increase in CGRP containing nerve fibers at 1 and 2day postinjury was noted subjacent to the injury site. In the 4day group, there were an extensive increase in the number of reactive fibers, followed by a partial return toward normal levels at 7~10 day postinjury, and return by 21days. 3. The sprouting of the CGRP containing nerve fibers was evident within 2day after dentinal injury, and by 4days there was a maximal increased, but was decreased at 7days and returned to normal 10~21 day postinjury. 4. In confocal laser scanning microscopic exammination, the distinct distribution pattern and sprouting reaction of CGRP containing nerve fibers were observed in stereoscopic images and three dimentional images. These results suggest that CGRP containing nerve fiber can be important role in the response to dental injury and pain regulation.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.34 no.5
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• pp.563-569
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• 2001

In order to utilize the processing wastes of squid, chitosan was prepared by intermittent deacetylation treaoent of $\beta-chitin$ contained richly in the pen of squid. Acetylchitosan also was synthesized from squid pen chitosan with anhydrous acetic acid and their characteristics were investigated. The amounts of nitrogen and ash of squid pen chitosan were $5.80.2\% and 0.2\pm0.03\%$ respectively, the yield of squid pen chitosan was $25\pm3\%$, the degree of deacetylation was $92\%$, and the molecular weight was $1.15\times10^6$, Acetyl contents of N-acetylchitosan powder, acetylchitosan bead, N-ACF-1 (N-acetylchitosan film-1) and N-ACF-2 (N-acetylchitosan film-2) were $55.9\%, 63.2\%, 56\% and 58.7\%$ respectively. Two major peaks, amide I ($1,653 cm^{-1}$) and II ($1,558 cm^{-1}$) bent, on FT-IR spectra of the N-acetylchitosan from squid pen were almost similar to these of $\beta-chitin$, While there was a broad single peak at $1,601 cm^{-1}$assigned to be an amide I bend in squid pen chitosan. The CP/MAS NMR spectra of $\beta-chitin$, squid pen chitosan and N-acetylchitosan from squid pen showed a relative broad and single peak at 74 ppm assigned to fifth carbon (C-5) and third carbon (C-3). In case of $\beta-chitin$ and N-acetylchitosan from squid pen, single peak at 74 ppm was showed as the same of $\beta-chitin$ type.