• Journal of Food Hygiene and Safety
• /
• v.34 no.2
• /
• pp.148-157
• /
• 2019

An optimized analytical method for sodium iron chloriphyllin in foods was established and verified by using high performance liquid chromatography with attached diode array detection. An Inertsil ODS-2 column and methanol-water (80:20 containing 1% acetate) as a mobile phase were employed. The limit of detection and quantitation of sodium iron chloriphyllin were 0.1 and 0.3 mg/kg, respectively, and the linearity of calibration curve was excellent ($R^2=0.9999$). The accuracy and precision were 93.9~104.95% and 2.0~7.7% in both inter-day and intra-day tests. Recoveries for candy and salad dressing were ranged between 93 and 104% (relative standard deviation, (RSD) 0.3~4.3%), and between 83 and 115% (RSD 1.2~2.0%), respectively. Liquid chromatography mass spectrometry was used to verify the main components of sodium iron chlorophyllin which were Fe-isochlorin e4 and Fe-chlorin e4.

• Journal of Food Hygiene and Safety
• /
• v.38 no.5
• /
• pp.319-331
• /
• 2023

Aminoglycoside antibiotics, also known as aminoglycosides (AGs), are veterinary drugs effective against a wide range of gram-negative and gram-positive bacteria. Owing to their recent use in cultured meats, it has become essential to establish an analytical method for safety management. AGs are highly polar compounds, and ion-pair reagents (IPRs) are used to ensure component separation. Owing to the high possibility of potential mechanical problems resulting from IPR addition to the mobile phase, an analytical method in which IPRs are added directly to the vial was explored. In this study, methods for analyzing 10 AGs via liquid chromatography-tandem mass spectrometry (LC-MS/MS) with the addition of two IPRs were validated for selectivity, detection limit, quantitation limit, recovery, and precision. The detection limit was 0.0001-0.0038 mg/kg, the quantification limit was 0.004-0.011 mg/kg, and the linearity (R²) within the concentration range of 0.01-0.5 mg/kg was over 0.99. Recovery and precision (expressed as relative standard deviation) evaluated in the two matrices (beef and cell culture media) ranged from 70.7% to 120.6% and 0.2% to 24.7%, respectively. The validated AG analytical method was then applied to 15 meats prepared from chicken, beef, and pork, and 6 culture media and additives used in cultured meat. No AGs were detected in any of the 15 meats distributed in Korea; however, streptomycin and dihydrostreptomycin were detected at levels ranging from 695.85 to 1152.71 mg/kg and 6.35 to 11.11 mg/kg, respectively, in the culture media additives. The LC-MS/MS method coupled with direct addition of IPRs to the vial can provide useful basic data for AG analysis and safety evaluation of meats as well as culture media and additives for cultured meats.

• 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.

• Korean Journal of Environmental Agriculture
• /
• v.36 no.3
• /
• pp.201-210
• /
• 2017

BACKGROUND: The current study was to monitor of 9 veterinary antibiotics (ceftiofur, clopidol, florfenicol, sulfamethazine, sulfamethoxazole, sulfathiazole, tetracycline, tiamulin, and tylosin) in manure using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive and negative electrospray ionization mode. METHODS AND RESULTS: Sample preparation was carried out using Mcllvaine buffer and citrate salts to adjust the pH of the sample followed by purification with dispersive solid phase extraction (d-SPE). Separation of analytes during LC-MS/MS analysis was conducted using an Eclipse Plus $C_{18}$ column and the mobile phase was in gradient mode with, 0.1% formic acid and 5 mM ammonium formate in methanol (A) and 0.1% formic acid and 5 mM ammonium formate in distilled water (B). The linearity of the matrix-matched calibrations of all tested antibiotics was good, with $R^2$ determination coefficients ${\geq}0.9920$. The limit of detection (LOD) and quantifications (LOQ) were $0.1-67.0{\mu}g/kg$ and $0.4-200.0{\mu}g/kg$, respectively. Analysis of 13 solid and liquid manure samples taken from the Republic of Korea revealed concentrations less than $0.7{\mu}g/kg$ for tiamulin, $1497.6{\mu}g/kg$ for sulfamethazine. CONCLUSION: To monitor 9 veterinary antibiotics from manure samples in 13 provincial areas throughout the Republic of Korea, an analytical method was developed. The developed method was fully validated and successfully applied for monitoring various veterinary antibiotics in manure samples.

• Korean Journal of Environmental Agriculture
• /
• v.36 no.3
• /
• pp.154-160
• /
• 2017

BACKGROUND:This study was carried out to establish an efficient sample preparation for the simultaneous determination of bisphenols (BPs) in river water samples using gas chromatography-mass spectrometry (GC-MS). Sample preparation was examined with conventional extraction methods, such as solid-phase extraction (SPE) and liquid-liquid extraction (LLE), and their efficiency was compared with validation results, including linearity of calibration curve, method detection limit (MDL), limit of quantification (LOQ), accuracy, and precision. METHODS AND RESULTS:The BPs (bisphenol A, BPA; bisphenol B, BPB; bisphenol C, BPC; bisphenol E, BPE; bisphenol F, BPF; bisphenol S, BPS) were analyzed using GC-MS. The range of MDLs by SPE and LLE methods was $0.0005{\sim}0.0234{\mu}g/L$ and $0.0037{\sim}0.2034{\mu}g/L$, and that of LOQs was $0.0015{\sim}0.0744{\mu}g/L$ and $0.0117{\sim}0.6477{\mu}g/L$, respectively. The calibration curve obtained from standard solution of $0.004{\sim}4.0{\mu}g/L$ (SPE) and $0.016{\sim}16{\mu}g/L$ (LLE) showed good linearity with $r^2$ value of 0.9969 over. Accuracy was 93.2~108% and 97.4~120%, and precision was 1.7~4.6% and 0.7~6.5%, respectively. The values of MDL and LOQ resulted from the SPE method were higher than those from the LLE method, particularly those values of BPA were highest among the BPs. Based on the results, the SPE method was applied to determine the BPs in river water samples. Water samples were collected from mainstream, tributary and sewage wastewater treatment plants (SWTPs) in the Yeongsan river basin. The concentration of BPB, BPC, BPE, BPF and BPS were not detected in all sites, whereas BPA was ranged $0.0095{\sim}0.2583{\mu}g/L$, which was $0.0166{\sim}0.0810{\mu}g/L$ for mainstreams, $0.0095{\sim}0.2583{\mu}g/L$ for tributaries, $0.0352{\sim}0.1217{\mu}g/L$ for SWTPs. CONCLUSION: From these results, the SPE method was very effective for the simultaneous determination of BPs in river water samples using GC-MS. We provided that it is a convenient, reliable and sensitive method enough to monitor and understand the fate of the BPs in aquatic ecosystems.

• Journal of Korean Society of Environmental Engineers
• /
• v.32 no.5
• /
• pp.443-454
• /
• 2010

Phthalate compounds are widely used as plasticizers in polyvinyl chlororide (PVC) resins and other industrial consumer products, and some of them are known to be endocrine disruptors. In Korea, a number of studies have been carried out for the measurement of phthalates in consumer products and drinking water. However, no data are available for those compounds in the ambient air where the general public are routinely exposed. In this study, we evaluated sampling and analytical methods for the determination of phthalates in the ambient atmosphere. A wide range of phthalates compounds were included in the target analytes, which are dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-butyl phthalate (DBP), butyl benzyl phthalate (BBP), di(2-ethylhexyl) phthalate (DEHP), and di-n-octyl phthalate (DOP). Most of samples were collected using a high volume sampler with a PUF/XAD-2 column/quartz fiber filter and then analyzed by GC/MS. Some of samples were simultaneously collected on XAD-2 using a low-volume sampler, together with high-volume samples. The analytical method applied in this study showed good repeatability and linearity. Quantitative detection limits were estimated from 0.60 to 17.84 ng/$m^3$ in air, depending on individual compounds. The field measurements were carried out at 3 sites located in Sihwa- Banwall industrial areas and a suburban area from January 2007 to November 2007. From the field experiments, DEHP, DMP and DBP appeared to be the most abundant compounds in the ambient air. It was also found that DMP, DEP and DBP were mainly distributed in the vapor phase, while BBP, DEHP and DOP were predominantly associated with the particulate phase. The concentrations of DEHP and DMP in the industrial areas ranged from 45.7 to 1,012.7 ng/$m^3$ and from 7.7 to 375.1 ng/$m^3$, respectively. Overall, the high-volume sampling method was demonstrated to be superior to the low-volume method for the determination of phthalates in the ambient atmosphere.

• Journal of Biomedical Engineering Research
• /
• v.25 no.4
• /
• pp.261-268
• /
• 2004

Osteoporosis is a clinical condition in which the amount of bone tissue is reduced and the likelihood of fracture is increased. It is known that the electrical property of the bone is related to its density, and, in particular, the electrical resistance of the bone decreases as the bone loss increases. This implies that the electrical property of bone may be an useful parameter to diagnose osteoporosis, provided that it can be readily measured. The study attempted to evaluate the electrical conductivity of bone using a technique of electrical impedance tomography (EIT). It nay not be easy in general to get an EIT for the bone due to the big difference (an order of 2) of electrical properties between the bone and the surrounding soft tissue. In the present study, we took an adaptive mesh regeneration technique originally developed for the detection of two phase boundaries and modified it to be able to reconstruct the electrical conductivity inside the boundary provided that the geometry of the boundary was given. Numerical simulation was carried out for a tibia phantom, circular cylindrical phantom (radius of 40 mm) inside of which there is an ellipsoidal homeogenous tibia bone (short and long radius are 17 mm and 15 mm, respectively) surrounded by the soft tissue. The bone was located in the 15 mm above from the center of the circular cross section of the phantom. The electrical conductivity of the soft tissue was set to be 4 mS/cm and varies from 0.01 to 1 ms/cm for the bone. The simulation considered measurement errors in order to look into its effects. The simulated results showed that, if the measurement error was maintained less than 5 %, the reconstructed electrical conductivity of the bone was within 10 % errors. The accuracy increased with the electrical conductivity of the bone, as expected. This indicates that the present technique provides more accurate information for osteoporotic bones. It should be noted that tile simulation is based on a simple two phase image for the bone and the surrounding soft tissue when its anatomical information is provided. Nevertheless, the study indicates the possibility that the EIT technique may be used as a new means to detect the bone loss leading to osteoporotic fractures.

• Korean Journal of Food Science and Technology
• /
• v.36 no.1
• /
• pp.14-18
• /
• 2004

Analysis methods of artificial sweeteners, aspartame, acesulfame potassium, sodium saccharin, and sucralose isolated from foods were developed using high performance liquid chromatography, HPLC conditions for aspartame, acesulfame potassium, and sodium saccharin were: column, Symmetry $C_{18}(3.9mm\;i.d{\times}150mm,\;5{\mu}m)$; mobile phase, 0.05M sodium phosphate monobasic : acetonitrile (9 : 1, pH 3.5, containing 0.01M tetrapropylammonium hydroxide); detector, UV detector at 210 nm. HPLC condition for sucralose were : column, Symmetry $C_{18}(3.9mm\;i.d{\times}150mm,\;5{\mu}m)$; mobile phase, water:methanol (7 : 3); detector, refractive index detection (sensitivity = 16). Recoveries of artificial sweeteners in foods including soft drinks, fruit and vegetable beverages, alcoholic beverages, fermented milk beverages, soybean milk, ice cream, snacks, chewing gums, jam, honey, kimchi salted food, special dietary products, processed fish products, candies, food additive mixtures, chocolate and cocoa were 76.1-101.3%, 82.3-103.2%, 83.1-103.7%, and 80,6-99.5% for aspartame, acesulfame potassium, sodium saccharin, and sucralose, respectively.

• Maxillofacial Plastic and Reconstructive Surgery
• /
• v.22 no.2
• /
• pp.164-173
• /
• 2000

The p16 protein is a cyclin dependent kinase inhibitor that inhibits cell cycle progression from $G_1$ phase to S phase in cell cycle. Many p16 gene mutations have been noted in many cancer-cell lines and in some primary cancers, and alterations of p16 gene function by DNA methylation have been noticed in various kinds of cancer tissues and cell-lines. There have been a large body of literature has accumulated indicating that abnormal patterns of DNA methylation (both hypomethylation and hypermethylation) occur in a wide variety of human neoplasma and that these aberrations of DNA methylation may play an important epigenetic role in the development and progression of neoplasia. DNA methylation is a part of the inheritable epigenetic system that influences expression or silencing of genes necessary for normal differentiation and proliferation. Gene activity may be silenced by methylation of up steream regulatory regions. Reactivation is associated with demethylation. Although evidence or a high incidence of p16 alterations in a variety of cell lines and primary tumors has been reported, that has been contested by other investigators. The precise mechanisms by which abnormal methylation might contribute to carcinogenesis are still not fully elucidated, but conceivably could involve the modulation of oncogene and other important regulatory gene expression, in addition to creating areas of genetic instability, thus predisposing to mutational events causing neoplasia. There have been many variable results of studies of head and neck squamous cell carcinoma(HNSCC). This investigation was studied on 13 primary HNSCC for p16 gene status by protein expression in immunohistochemistry, and DNA genetic/epigenetic analyzed to determine the incidence, the mechanisms, and the potential biological significance of its Inactivation. As methylation detection method of p16 gene, the methylation specific PCR(MSP) is sensitive and specific for methylation of any block of CpG sites in a CpG islands using bisulfite-modified DNA. The genomic DNA is modified by treatment with sodium bisulfate, which converts all unmethylated cytosines to uracil(thymidine). The primers designed for MSP were chosen for regions containing frequent cytosines (to distinguish unmodified from modified DNA), and CpG pairs near the 5' end of the primers (to provide maximal discrimination in the PCR between methylated and unmethylated DNA). The two strands of DNA are no longer complementary after bisulfite treatment, primers can be designed for either modified strand. In this study, 13 paraffin embedded block tissues were used, so the fragment of DNA to be amplified was intentionally small, to allow the assessment of methylation pattern in a limited region and to facilitate the application of this technique to samlples. In this 13 primary HNSCC tissues, there was no methylation of p16 promoter gene (detected by MSP and automatic sequencing). The p16 protein-specific immunohistochemical staining was performed on 13 paraffin embedded primary HNSCC tissue samples. Twelve cases among the 13 showed altered expression of p16 proteins (negative expression). In this study, The author suggested that low expression of p16 protein may play an important role in human HNSCC, and this study suggested that many kinds of genetic mechanisms including DNA methylation may play the role in carcinogenesis.

• Korean Journal of Agricultural Science
• /
• v.11 no.2
• /
• pp.233-243
• /
• 1984

The present study was carried out to determine the changes of the sex hormone levels in serum throughout the estrous cycle and the gestation period on the Landrace gilts. The blood samples were taken from the vein of six gilts. LH, FSH, prolactin, progesterone, $estradiol-17{\beta}$ and cortisol in serum were analyzed by the radioimmunoassay methods. The results obtained on this study were summarized as follows; 1. The age at puberal estrus was 179.5 days, the weight at puberal estrus was 88.2kg, the length of estrous cycle was 21.3days, the gestation length was 114days and the litter size was 9.5 head in the Landrace gilts. 2. During the estrous cycle, the serum LH and prolactin concentrations were below 1.56mIU/ml and 2.4ng/ml, respectively, under the limit of detection of the assay. The FSH concentrations ranged from 1.50 to 2.20mIU/ml for day 6~15 after the estrus and they were below 1.25mIU/ml from day 3 to day + 3, with day 0 being the first day of the estrus. 3. Progesterone concentrations were 1.90ng/ml at day 0 of the estrus and increased about 13.1ng/ml at day 3 of the estrus, and reached peak levels at day 9. $Estradiol-17{\beta}$ concentrations were below 27.2pg/ml throughout the luteal phase, and reached about 27.2pg/ml at day 0 and day 18. Cortisol concentrations reached peak levels at dey 0 and ranged from 24.65 to 28.57ng/ml throughout the luteal phase. 4. During the gestation period, the concentrations of LH, FSH and prolactin ranged of 3.10~4.37mIU/ml, 1.30~1.80mIU/ml and 2.60~6.70ng/ml, respectively. 5. Progesterone concentrations declined from 38.90~16.85ng/ml throughout the pregnancy to 1.90ng/ml at the time of parturition. $Estradiol-17{\beta}$ concentrations increased from 27.20pg/ml at 15 days after the pregnancy to 620.17pg/ml at the time of parturition. Cortisol concentrations reached peak levels at the time of parturition and ranged from 13.58 to 22.31ng/ml throughout the pregnancy.