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β-Carotene Content in Selected Agricultural Foods (조미료류, 채소류, 과일류 등의 농산식품에 함유된 베타카로틴 함량 분석)

  • Shin, Jung-Ah;Choi, Youngmin;Lee, Ki-Teak
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.44 no.3
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    • pp.418-424
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    • 2015
  • The content of ${\beta}$-carotene in agricultural foods, such as seasonings, tea, vegetables, cereals, nuts & seeds, oils & fats, and fruits, were quantitatively analyzed using reversed-phase HPLC with an UV/visible detector. Standard reference material (SRM) 2385 was used as a control material to validate measurement of ${\beta}$-carotene in this study. Recovery percentage and relative standard deviation of ${\beta}$-carotene in SRM 2385 were 102% and 1.73%, respectively. Vegetables and tea contained relatively high concentrations of ${\beta}$-carotene (young barley powder, $17,293.95{\mu}g/100g$; raw young barley, $2,755.15{\mu}g/100g$; dried green tea leaves, $13,671.85{\mu}g/100g$; green tea powder, $7,579.04{\mu}g/100g$). Contents of ${\beta}$-carotene in nuts & seeds as well as oils & fats ranged from $11.32{\mu}g/100g$ in almond products (roasted with salt) to $58.56{\mu}g/100g$ in perilla seed oil. Among 20 fruits, a high content of ${\beta}$-carotene was found in apricots (raw), which contained $2,280.35{\mu}g/100g$.

Analysis and verification of vitamin B12 in animal foods for update of national standard food composition table (국가표준식품성분표 개정을 위한 동물성 식품 비타민 B12 분석 및 검증)

  • Jeong, Yon Na;Park, Su-Jin;Lee, Sang Hoon;Choi, Youngmin;Choi, Kap Seong;Chun, Jiyeon
    • Korean Journal of Food Science and Technology
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    • v.52 no.4
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    • pp.317-324
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    • 2020
  • In order to create the national food nutrient database, a total of 41 animal foods (ham, seafood, edible insects and eggs) were analyzed for their vitamin B12 content and the applied immunoaffinity-HPLC was verified. Ham vitamin B12 contents were 0.30-0.65 ㎍/100 g. Seafood showed relatively high vitamin B12 level, where the values of fermented clam were the highest (26.80 ㎍/100 g) followed by fermented pollack roe. Vitamin B12 was not detected in silkworm pupae and beetles, while relatively high levels were found in the two-spotted cricket imago (6.70 ㎍/100 g). Chicken and quail egg yolk had roughly 100- and 30-times higher vitamin B12 levels as compared to their egg white. Vitamin B12 contents in quail and chicken eggs were significantly enhanced by boiling (p<0.05). Results based on accuracy (97-102% recovery) and precision (<5% RSD) indicate that this study provides reliable vitamin B12 information on animal foods consumed in Korea.

Qualitative and quantitative PCR detection of insect-resistant genetically modified rice Agb0101 developed in korea (해충저항성 유전자변형 벼 Agb0101에 대한 PCR 검정)

  • Shin, Kong-Sik;Lee, Jin-Hyoung;Lim, Myung-Ho;Woo, Hee-Jong;Qin, Yang;Suh, Seok-Cheol;Kweon, Soon-Jong;Cho, Hyun-Suk
    • Journal of Plant Biotechnology
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    • v.40 no.1
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    • pp.18-26
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    • 2013
  • Genetically modified (GM) rice Agb0101, which expresses the insecticidal toxin modified cry1Ac (mcry1Ac1) gene, was developed by the Rural Development Administration in Korea. To monitor the probable release of Agb0101 in the future, it is necessary to develop a reliable detection method. Here, we developed the PCR detection method for monitoring and tracing of GM rice. The primer pair (RBEgh-1/-2) from a starch branching enzyme (RBE4) gene was designed as an endogenous reference, giving rise to an expected PCR amplicon of 101 bp. For the qualitative PCR detection, construct- and event-specific primers were designed on the basis of integration sequence of T-DNA. Event-specific PCRs amplified specifically 5'- or 3'-junction region spanning the native genome DNA and the integrated gene construct, while none of amplified product was shown on crops, rice varieties, and other insect-resistant transgenic rice lines. The event-specific real-time PCR method was performed using TaqMan probe and plasmid pRBECrR containing both rice endogenous gene RBE4 sequence and 5'-junction sequence as the reference molecule. The absolute limit of quantification (LOQ) of real-time PCR was established with around 10 copies for one plasmid molecule pRBECrR. Thereafter, the different amounts of transgenic rice (1, 3, 5, and 10%, respectively) were quantified by using the established real-time PCR method, with a range below 19.55% of the accuracy expressed as bias, 0.06-0.40 of standard deviation (SD) and 3.80-7.01% of relative standard deviations (RSD), respectively. These results indicate that the qualitative and quantitative PCR methods could be used effectively to detect the event Agb0101 in monitoring and traceability.

Establishment of an Analytical Method for Determination of Fungicide Oxathiapiprolin in Agricultural Commodities using HPLC-UV Detector (HPLC-UVD를 이용한 농산물 중 살균제 Oxathiapiprolin의 잔류분석법 확립)

  • Jang, Jin;Kim, Heejung;Do, Jung Ah;Ko, Ah-Young;Lee, Eun Hyang;Ju, Yunji;Kim, Eunju;Chang, Moon-Ik;Rhee, Gyu-Seek
    • Journal of Food Hygiene and Safety
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    • v.31 no.3
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    • pp.186-193
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    • 2016
  • An analytical method was developed for the determination of oxathiapiprolin in agricultural commodities. Oxathiapiprolin is a new oomycide (fungicide of piperidinyl thiazole isoxazoline class) which controls downy mildew in cucurbits caused by Pseudoperonospora cubensis (oomycete plant pathogen). Agricultural commodities were extracted with acetonitrile and partitioned with dichloromethane to remove the interference, adjusting pH between 9 and 10 by 1 N sodium hydroxide. After purification by silica SPE cartridge to clean up the interference of organic compounds, they were finally quantified by HPLC-UVD (high performance liquid chromatograph ultraviolet detector) using a wavelength at 260 nm and confirmed by LC-MS (liquid chromatograph mass spectrometer) in electro-spray ionization positive ion mode. The standard calibration curve was linear with coefficients of determination ($r^2$) 1.00 over the calibration ranges (0.025-2.5 mg/L). Recoveries were ranged between 86.7 to 112.7%, with relative standard deviations less than 10% at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates. The overall results were determined and estimated according to the CODEX guidelines (CAC/GL40). The proposed method for determination of oxathiapiprolin residues in agricultural commodities can be used as an official method.

Determination of aromatic amino acids by chemiluminometric assay with Luminol-H2O2-Cu(II) system (Luminol-H2O2-Cu(II) 시스템을 이용한 방향족 아미노산의 화학발광법적 정량)

  • Kim, Kyung-Min;Kim, Young-Ho;Lee, Sang-Hak
    • Analytical Science and Technology
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    • v.25 no.3
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    • pp.171-177
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    • 2012
  • A determination method of aromatic amino acids such as trytophan (Trp), tyrosine (Tyr), and phenylalanine (Phe) using luminol-$H_2O_2$-Cu(II) system has been presented. In the presence of an aromatic amino acid, the enhanced chemiluminescence (CL) intensity of luminol-$H_2O_2$-Cu(II) system was obtained by forming a complex between Cu(II) and the amino acid. Based on the above phenomenon, a sensitive and fast determination of three aromatic amino acids was performed using the CL method in batch-type detection system. To optimize determination conditions, the kinetic influence of an aromatic amino acid on the luminol-$H_2O_2$-Cu(II) system and the effects of $H_2O_2$ and Cu(II) concentration, pH, and buffers were investigated. Under the optimized conditions, the calibration curve was linear over the range from $1.0{\times}10^{-6}$ to $2.0{\times}10^{-5}\;M$ for Trp, $1.0{\times}10^{-6}$ to $2.0{\times}10^{-5}\;M$ for Try, and $2.0{\times}10^{-6}$ to $2.0{\times}10^{-5}\;M$ for Phe, respectively. In this range, reproducibility (RSD, n = 4) of Trp, Try, and Phe were 3.21%, 2.64%, and 2.48%, respectively. The limit of detection ($3{\sigma}/s$) was calculated to be $6.8{\times}10^{-7}\;M$ for Trp, $5.7{\times}10^{-7}\;M$ for Try, and $9.6{\times}10^{-7}\;M$ for Phe.

Residue analysis of penicillines in livestock and marine products (국내 유통 축·수산물 중 페니실린계 동물용의약품에 대한 잔류실태조사)

  • Song, Ji-Young;Hu, Soo-Jung;Joo, Hyun-Jin;Kim, Mi-Ok;Hwang, Joung-Boon;Han, Yoon-Jung;Kwon, Yu-Jihn;Kang, Shin-Jung;Cho, Dae-Hyun
    • Analytical Science and Technology
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    • v.25 no.4
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    • pp.257-264
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    • 2012
  • Penicillins belong to the ${\beta}$-lactam class of antibiotics, and are frequently used in human and veterinary medicine. Despite the positive effects of these drugs, improper use of penicillins poses a potential health risk to consumers. This study has been undertaken to determinate multi-residues of penicillins, including amoxicillin, ampicillin, oxacillin, bezylpenicillin, cloxacillin, dicloxacillin, and nafcillin, using liquid chromatographic tandem mass spectrometer (LC-MS/MS). The developed method was validated for specificity, precision, recovery, and linearity in livestock and marine products. The analytes were extracted with 80% acetonitrile and clean-up by a single reversed-phase solid-phase extraction step. Six penicillins presented recoveries higher than 76% with the exception of Amoxicillin. Relative standard deviations (RSDs) were not more than 10%. The method was applied to 225 real samples. Benzylpenicillin was detected in 12 livestock products and 7 marine products. Amoxicillin, ampicillin, cloxacilllin, dicloxacillin, nafcillin and oxacillin were not detected. The detected levels were 0.001~0.009 mg/kg in livestock products excluding eggs and milk. In marine products, the detected levels were under 0.03 mg/kg. They were under the MRL levels. As monitoring results, it is identified to be safe but it is considered that safety management of antibiotics should continue by monitoring.

Shoulder Uptake in the Bone Scintigraphy in Patients with Hemiplegic Reflex Sympathetic Dystrophy Syndrome (반신마비성 반사성교감신경 이영양증후군 환자의 골스캔상 견관절 섭취)

  • Lee, Jong-Jin;Chung, June-Key;Lee, Dong-Soo;Hong, Joon-Beom;Han, Tai-Ryoon;Lee, Myung-Chul
    • The Korean Journal of Nuclear Medicine
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    • v.38 no.4
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    • pp.288-293
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    • 2004
  • Purpose: increased uptake of wrist and hand joints in three phase bone scintigraphy (TPBS) have been used in the detection of reflex sympathetic dystrophy syndrome (RSDS). TPBS frequently shows increased shoulder uptake in the hemiplegic RSDS patients. We investigated the significance of the shoulder uptake in the detection of these patients. Materials and Methods: Twenty three patients who had hemiplegia due to brain stroke and diagnosed as RSD were enrolled in this study (M:F=16:7, R:L=11:12). The mean age was $63{\pm}10$ yrs. Ter normal volunteer (mean age: $60{\pm}5$, M:F=1:9) data was used as control group. TPBS was performed $59{\pm}32$ days after stoke (acute stage). We obtained the count ratios of bilateral hands by drawing a region of interest (ROI) in three phase images and compared to the count ratios of shoulders in the delayed image. Hand ROI included an ipsilateral wrist. Sensitivity of detecting the affected limb was defined using the right/left count ratio of normal control. Results: Sensitivities using count ratios of hand blood flow, blood pool and delayed image were 45%, 76% and 78%, respectively. Sensitivity of shoulder count ratio was 74%. Log of right/left counts of hand delayed image and that of shoulder delayed image were correlated well with statistical significance (Spearman's R=0.824, p<0.001). Conclusion: Shoulder uptake showed good correlation with hand uptake in the delayed image of TPBS. Shoulder uptake maybe helpful in the diagnosis of reflex sympathetic dystrophy syndrome in patients with hemiplegia.

Simultaneous HPLC Determination of Marker Compounds for the Standardization of Hedyotis diffusa (백운풀의 지표성분 설정 및 품질표준화를 위한 정량 분석법)

  • Bang, Han-Yeol;Yang, Eun-Ju;Kim, Jeong-Ah;Song, Kyung-Sik
    • Journal of Life Science
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    • v.23 no.8
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    • pp.1025-1031
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    • 2013
  • From a 95% ethanolic extract of H. diffusa, four marker compounds (HD1~HD4) were isolated, which were relatively unique and exist in comparably high contents. The structures of marker compounds were identified as digitolutein (1), 2-hydroxy-3-methylanthraquinone (2), (E/Z)-6-O-p-coumaroyl scandoside methyl ester (4:1 mixture) (3), and (E/Z)-6-O-p-methoxycinnamoyl scandoside methyl ester (4:1 mixture) (4), respectively, on the basis of $^{13}C$ and $^1H$-NMR analyses. The calibration curves of marker compounds showed high linearity, as their correlation coefficient ($R^2$) were in the range of 0.9991~0.9999. In addition, the limit of detection (LOD) and the limit of quantification (LOQ) were $0.03{\sim}0.07{\mu}g/ml$ and $0.099{\sim}0.231{\mu}g/ml$, respectively. The intra-day/inter-day precision and accuracy were 0.23~2.00%/0.25~1.16% and 94.60~108.44%/94.73-110.23%, respectively. The optimal HPLC conditions for the simultaneous quantification of HD1~HD4 were as follows: stationary phase; Merck Chromolith RP-18e ($100{\times}4.6mm$, $5{\mu}m$), column temp.; room temperature, UV detection at 280 nm, flow rate; 2.0 ml/min, injection volume; $10{\mu}l$, mobile phase; start with the mixture of 80% solvent A ($H_2O$ containing 0.5% acetic acid) and 20% solvent B (methanol containing 0.5% acetic acid) and gradually decrease solvent A to 40% in 9 min., then retain this condition to 18 min. Under the HPLC condition, the four marker compounds 1~4 were successfully separated without any interference of other constituents. The results obtained in this study are expected to be helpful for the development of nutraceutics and natural medicines and for the quality control of this plant.

Simultaneous Determination of Water Soluble Vitamins B Group in Health Functional Foods etc. by HPLC (건강기능식품 등 중 수용성 비타민 B군의 HPLC를 이용한 동시분석법)

  • Kim, Seon Hee;Kim, Jae-Hyun;Lee, Hwa Jung;Oh, Jae Myoung;Lee, Sung Hye;Bahn, Kyeong Nyeo;Seo, Il Won;Lee, Young Joo;Lee, Jin Hee;Kang, Tae Seok
    • Journal of Food Hygiene and Safety
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    • v.30 no.2
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    • pp.143-149
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    • 2015
  • This study was conducted to simultaneous analysis methods for water soluble vitamins B group (vitamin $B_1$, vitamin $B_2$, nicotinic acid, nicotinamide, vitamin $B_6$) which is used as health functional foods etc. Analytical methods of water-soluble vitamins B group by HPLC were established through instrumental analytical conditions, and the examination of data such as domestic and foreign reliable methods, and papers of journal. HPLC method analyzing water soluble vitamins B group was established using Capcell Pak C18 UG 120 column in 270 nm through test of columns. The validation has been performed on the method to determine linearity, accuracy, limits of quantification (LOQ) and repeatability for water soluble vitamins B group. An excellent linearity ($r^2=0.999$) was observed for vitamin $B_1$, vitamin $B_2$, nicotinic acid, nicotinamide, vitamin $B_6$ in the concentration range ($0.1{\sim}2{\mu}g/mL$). Observed recovery of vitamin $B_1$ was found to be between 100 and 103%, vitamin $B^2$ was found to be between 104 and 112%, nicotinic acid was found to be between 82 and 85%, nicotinamide was found to be between 121 and 124% and vitamin $B_6$ was found to be between 95 and 104%. LOQ of vitamin $B_1$ was found to be $0.04{\mu}g/mL$, vitamin $B_2$ was found to be $0.05{\mu}g/mL$, nicotinic acid was found to be $0.15{\mu}g/mL$, nicotinamide was found to be $0.08{\mu}g/mL$ and vitamin $B_6$ was found to be $0.63{\mu}g/mL$. Repeatability precision for vitamin $B_1$ was found to be 0.4%, vitamin $B_2$ was found to be 0.4%, nicotinic acid was found to be 0.5%, nicotinamide was found to be 0.7% and vitamin $B_6$ was found to be 0.4% relative standard deviation (RSD). Also, verify the accuracy of the simultaneous analysis methods, we monitored the labeled contents of the health functional foods and children's preferred foods.

Establishment of Choline Analysis in Infant Formulas and Follow-up Formulas by Ion Chromatograph (이온크로마토그래프를 이용한 조제유류 및 영아용·성장기용 조제식 중 콜린 함량 분석법 연구)

  • Hwang, Kyung Mi;Ham, Hyeon Suk;Lee, Hwa Jung;Kang, Yoon Jung;Yoon, Hae Seong;Hong, Jin Hwan;Lee, Hyoun Young;Kim, Cheon Hoe;Oh, Keum Soon
    • Journal of Food Hygiene and Safety
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    • v.32 no.5
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    • pp.411-417
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    • 2017
  • This study was conducted to establish the analysis method for the contents of choline in infant formulas and follow-up formulas by ion chromatograph (IC). To optimize the method, we compared several conditions for extraction, purification and instrumental measurement using spiked samples and certified reference material (CRM; NIST SRM 1849a) as test materials. IC method for choline was established using Ion Pac CG column and 18 mM $H_2SO_4$ mobile phase. The parameters of validation were specificity, linearity, LOD, LOQ, recovery, accuracy, precision and repeatability. The specificity was confirmed by the retention time and the linearity, $R_2$ was over 0.999 in range of 0.5~10 mg/L. The detection limit and quantification limit were 0.14, 0.43 mg/L. The accuracy and precision of this method using CRM were 95%, 2.1% respectively. Optimized methods were applied in sample analysis to verify the reliability. All the tested products were acceptable contents of choline compared with component specification for nutrition labeling. The standard operating procedures were prepared for choline to provide experimental information and to strengthen the management of nutrient in infant formula and follow-up formula.