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Simultaneous Determination of Eight Sugar Alcohols in Foodstuffs by High Performance Liquid Chromatography (HPLC를 이용한 식품 중 당알코올 8종 동시분석)

  • Lim, Ho-Soo;Park, Sung-Kwan;Kwak, In-Shin;Kim, Hyung-Il;Sung, Jun-Hyun;Choi, Jung-Yoon;Kim, So-Hee
    • Journal of Food Hygiene and Safety
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    • v.26 no.1
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    • pp.16-24
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    • 2011
  • A method was established for the simultaneous determination of sugar alcohols, erythritol, xylitol, sorbitol, inositol, mannitol, maltitiol, lactitol and isomalt by High Performance Liquid Chromatography (HPLC). The sugar alcohols were converted into strong ultraviolet (UV)-absorbing derivatives with p-nitrobenzoyl chloride (PNBC). HPLC was performed on Imtakt Unison US-$C_18$ column, using acetonitrile: water (77:23) as a mobile phase and UV detection (260 nm). The calibration curves for all sugar alcohols tested were linear in the 10~200 mg/L range. The average recoveries of the sugar alcohols from three confectioneries spiked at 100 ppm of eight sugar alcohol standards ranged from 81.2 to 123.1% with relative standard deviations ranging fromo 0.2 to 4.9%. The limits of detection (LODs) were $0.5{\sim}8\;{\mu}g/L$ and the limits of quantification (LOQs) were $2{\sim}17\;{\mu}g/L$. Reproducibility of 8 sugar alcohols was 0.28~1.97 %RSD. The results of the analysis of confectioneries showed that 89 samples of 130 were detected and the sugar alcohols content of samples investigated varied between 0.4 and 693.7 g/kg. A method for the simultaneous determination of eight sugar alcohols will be used as basic data for control of sugar alcohols in confectioneries, and quality control in food manufacturing.

A Simultaneously Analytical Method of Phthalate and Adipate Plasticizers in Food Packaging by Dual-Column GC-FID System (Dual-Column GC-FID System을 이용한 식품 포장재 중 Phthalate류 및 Adipate류 가소제의 동시 분석법)

  • Kang Gil-Jin;Kwak In-Shin;Eom Mi-Ok;Jeon Dea-Hoon;Kim Hyung-il;Sung Jun-Hyun;Choi Jung-Mi;Kim Eun-Kyung;Lee Young Ja
    • Journal of Food Hygiene and Safety
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    • v.20 no.4
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    • pp.277-283
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    • 2005
  • A plasticizer is a substance which is added to a material to improve its processability, flexibility and stratchability. Phthalates and adipates are the most frequently used plasticizers of poly(vinyl chloride) (PVC). However, they can migtate into food from PVC food packaging, and some of them are especially suspected as endocrine disruptors. In this study, Simultaneous analysis of 13 phthalates and 9 adipates were carried out by dual-column gas chromatography system equipped wi two FID detectors for rapid confirmation and quantification. The Proposed method was validated with > 0.993 of linearity in the ranges of 10-500 mg/l, < $3.5\%$ RSD of reproducability in 10 inter-days sample preparations, and > $98.1\%$ of recoveries for all the plasticizers. DEHA was detected in all the 3 PVC wraps at levels of 176.9-198.5mg/g. Among the 51 samples of PVC gaskets, the targeted plasticizers were detected in 41 samples. Of these plasticizer detected samples,40 contained DIDP at the levels of 157.3-374.7 mg/g and one contained DMP at the levels of 165.6 mg/g. Also, some plasticizers were detected in other packaging materials such as PET, PP, PE, Pulp. But it might be attributed to contamination in manufacturing.

A Study on the Characteristics of Condensable Fine Particles in Flue Gas (배출가스 중 응축성미세먼지 특성 연구)

  • Gong, Buju;Kim, Jonghyeon;Kim, Hyeri;Lee, Sangbo;Kim, Hyungchun;Jo, Jeonghwa;Kim, Jeonghun;Gang, Daeil;Park, Jeong Min;Hong, Jihyung
    • Journal of Korean Society for Atmospheric Environment
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    • v.32 no.5
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    • pp.501-512
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    • 2016
  • The study evaluated methods to measure condensable fine particles in flue gases and measured particulate matter by fuel and material to get precise concentrations and quantities. As a result of the method evaluation, it is required to improve test methods for measuring Condensable Particulate Matter (CPM) emitted after the conventional Filterable Particulate Matter (FPM) measurement process. Relative Standard Deviation (RSD) based on the evaluated analysis process showed that RSD percentages of FPM and CPM were around 27.0~139.5%. As errors in the process of CPM measurement and analysis can be caused while separating and dehydrating organic and inorganic materials from condensed liquid samples, transporting samples, and titrating ammonium hydroxide in the sample, it is required to comply with the exact test procedures. As for characteristics of FPM and CPM concentrations, CPM had about 1.6~63 times higher concentrations than FPM, and CPM caused huge increase in PM mass concentrations. Also, emission concentrations and quantities varied according to the characteristics of each fuel, the size of emitting facilities, operational conditions of emitters, etc. PM in the flue gases mostly consisted of CPM (61~99%), and the result of organic/inorganic component analysis revealed that organic dusts accounted for 30~88%. High-efficiency prevention facilities also had high concentrations of CPM due to large amounts of $NO_x$, and the more fuels, the more inorganic dusts. As a result of comparison between emission coefficients by fuel and the EPA AP-42, FPM had lower result values compared to that in the US materials, and CPM had higher values than FPM. For the emission coefficients of the total PM (FPM+CPM) by industry, that of thermal power stations (bituminous coal) was 71.64 g/ton, and cement manufacturing facility (blended fuels) 18.90 g/ton. In order to estimate emission quantities and coefficients proper to the circumstances of air pollutant-emitting facilities in Korea, measurement data need to be calculated in stages by facility condition according to the CPM measurement method in the study. About 80% of PM in flue gases are CPM, and a half of which are organic dusts that are mostly unknown yet. For effective management and control of PM in flue gases, it is necessary to identify the current conditions through quantitative and qualitative analysis of harmful organic substances, and have more interest in and conduct studies on unknown materials' measurements and behaviors.

Analysis of Diflubenzuron in Agricultural Commodities by Multiresidue Method (동시 다성분 분석법에 의한 농산물 중 Diflubenzuron 분석)

  • Park, Sun-Hee;Han, Chang-Ho;Kim, Ae-Kyung;Shin, Jae-Min;Lee, Jae-Kyoo;Park, Young-Hae;Kim, Ji-Min;Hwang, Lae-Hong;Chang, Min-Su;Song, Mi-Ok;Park, Ju-Sung;Yun, Eun-Sun;Kim, Mu-Sang;Jung, Kweon
    • The Korean Journal of Pesticide Science
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    • v.18 no.4
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    • pp.269-277
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    • 2014
  • The multiclass pesticide multiresidue method for the simultaneous determination of diflubenzuron in agricultural products was conducted by using HPLC-UVD. The method was validated through the guidelines of linearity, specificity, limit of detection (LOD), limit of quantification (LOQ), accuracy and precision with pesticide-free spinach, Korean cabbage, eggplant, squash, sweet pepper, cucumber, Korean melon. The calibration curve of diflubenzuron was linear over the concentration range of 0.05-5 mg/kg with correlation coefficient of above 0.99999. The limit of detection and quantification was 0.008 and 0.02 mg/kg. Mean recoveries of diflubenzuron for each sample were 77.5-105.6%. Relative standard deviation (RSD) in recoveries were all less than 20%. The intra-day and inter-day precision (RSD) were 0.4-1.9% and 0.7-1.9%, respectively. The result of validation indicated that this method was accurate and rapid assay.

Validation of a Rapid Quantitative Method for the Residues of Nitrofuran Metabolites in Loach by Accelerated Solvent Extraction and HPLC Triple Quadrupole Mass Spectrometry

  • Ryu, Eun Chae;Han, Yun-jeong;Park, Seong-soo;Lim, Chul-joo;Choi, Sunok;Park, Se Chang
    • Journal of Food Hygiene and Safety
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    • v.31 no.2
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    • pp.85-93
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    • 2016
  • A rapid method using HPLC-MS/MS has been developed for quantitative determination of the metabolites of nitrofurans, namely 3-amino-2-oxazolidone (AOZ), 5-morpholinomethyl-3-amino-2-oxazolidinone (AMOZ), 1-ammino-hydantoin (AHD) and semicarbazide (SEM) in loach. The extraction procedure was founded on simultaneous acidic hydrolysis and derivatization using 2-nitrobenzaldehyde (2-NBA) for 1 hour at $50^{\circ}C$, followed by purification with liquid-liquid extraction. Recovery was evaluated by spiking standards into blank samples at three levels (0.5, 1.0 and $2.0{\mu}g/kg$), and the mean recovery was 75.1-108.1%. Precision values expressed as the relative standard deviation (%RSD) were ${\leq}8.7%$ and ${\leq}8.5%$ for intra-day and inter-day precision, respectively. Linearity was studied in the range of $0.2-20{\mu}g/Kg$ for NBAOZ, $0.8-20{\mu}g/Kg$ for NBAMOZ, $0.2-20{\mu}g/Kg$ for NBAHD, and $0.1-20{\mu}g/Kg$ for NBSEM, and the obtained coefficient correlations (r) were ${\geq}0.99$ for all compounds. Limits of detection (LODs) for the derivatized nitrofuran metabolites were established at $0.06{\mu}g/Kg$ for NBAOZ, $0.24{\mu}g/Kg$ for NBAMOZ, $0.06{\mu}g/Kg$ for NBAHD, and $0.03{\mu}g/Kg$ for NBSEM. Limits of quantification (LOQs) were established at $0.2{\mu}g/Kg$ for NBAOZ, $0.8{\mu}g/Kg$ for NBAMOZ, $0.2{\mu}g/Kg$ for NBAHD, and $0.1{\mu}g/Kg$ for NBSEM. This simplified rapid method for reducing the derivatization and hydrolysis times can be applied to the determination of nitro-furan residues in loach.

Method for Validation of Caffeoylquinic Acid Derivatives in Ligularia fischeri Leaf Extract as Functional Ingredients (건강기능식품 기능성 원료로서 곰취잎 추출물의 Caffeoylquinic Acid계 성분 분석법 검증)

  • Kwon, Jin Gwan;Kim, Jin Kyu;Seo, Changon;Hong, Seong Su;Ahn, Eun-Kyung;Seo, Dong-Wan;Oh, Joa Sub
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.45 no.1
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    • pp.61-67
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    • 2016
  • An HPLC analysis method was developed for standard determinations of chlorogenic acid, 3,4-di-O-caffeoylquinic acid, 3,5-di-O-caffeoylquinic acid, and 4,5-di-O-caffeoylquinic acid as functional health materials in Ligularia fischeri extract. HPLC was performed on a $C_{18}$ Kromasil column ($4.6{\times}250mm$, $5{\mu}m$ column) with a gradient elution of 0.1% (v/v) trifluoroacetic acid and acetonitrile at a flow rate of 1.0 mL/min at $30^{\circ}C$. The analytes were detected at 330 nm. The HPLC method was validated in accordance with the International Conference on Harmonization guideline of analytical procedures with respect to specificity, precision, accuracy, and linearity. The limits of detection and quantitation for the four compounds were 3.0~14.6 and $9.2{\sim}44.4{\mu}g/mL$, respectively. Calibration curves showed good linearity ($r^2$ > 0.999), and the precision of analysis was satisfied (less than 0.9%). Recoveries of quantified compounds ranged from 98.96 to 101.81%. This result indicates that the established HPLC method is very useful for the determination of marker compounds in Ligularia fischeri leaf extracts.

Identification of Flavonoids from Extracts of Opuntia ficus-indica var. saboten and Content Determination of Marker Components Using HPLC-PDA (손바닥선인장 추출물의 플라보노이드 구조 규명 및 HPLC-PDA를 이용한 지표성분의 함량 분석)

  • Park, Seungbae;Kang, Dong Hyeon;Jin, Changbae;Kim, Hyoung Ja
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.46 no.2
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    • pp.210-219
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    • 2017
  • This study aimed to establish an optimal extraction process and high-performance liquid chromatography (HPLC)-photodiode array (PDA) analytical method for determination of marker compounds, dihydrokaempferol (DHK) and 3-O-methylquercetin (3-MeQ), as a part of materials standardization for the development of health functional foods from stems of Opuntia ficus-indica var. saboten (OFS). The quantitative determination method of marker compounds was optimized by HPLC analysis, and the correlation coefficient for the calibration curve showed very good linearity. The HPLC-PDA method was applied successfully to quantification of marker compounds in OFS after validation of the method in terms of linearity, accuracy, and precision. Ethanolic extracts from stems of O. ficus-indica var. saboten (OFSEs) were evaluated by reflux extraction at 70 and $80^{\circ}C$ with 50, 70, and 80% ethanol for 3, 4, 5, and 6 h. Among OFSEs, OFS70E at $80^{\circ}C$ showed the highest contents of DHK and 3-MeQ of $26.42{\pm}0.65$ and $3.88{\pm}0.29mg/OFS100g$, respectively. Furthermore, OFSEs were determined for their antioxidant activities by measuring 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging and lipid peroxidation (LPO) inhibitory activities in rat liver homogenate. OFS70E at $70^{\circ}C$ showed the most potent antioxidant activities with $IC_{50}$ values of $1.19{\pm}0.11$ and $0.89{\pm}0.09mg/mL$ in the DPPH radical scavenging and LPO inhibitory assays, respectively. To identify active components of OFS, various chromatographic separation of OFS70E led to isolation of 11 flavonoids: dihydrokaempferol, dihydroquercetin, 3-O-methylquercetin, quercetin, isorhamnetin 3-O-glucoside, isorhamnetin 3-O-galactoside, narcissin, kaempferol 7-O-glucoside, quercetin 3-O-galactoside, isorhamnetin, and kaempferol 3-O-rutinoside. The results suggest that standardization of DHK in OFSEs using HPLC-PDA analysis would be an acceptable method for the development of health functional foods.

Development of Analysis Method of Gardenia Yellow as Natural Colorants and Content Survey in Commercial Foods by HPLC (HPLC를 이용한 천연착색료인 치자황색소의 분석법 개발 및 시판 식품중 함유량조사)

  • Kim, Hee-Yun;Kim, So-Hee;Hong, Ki-Hyoung;Lee, Chul-Won;Kim, Kil-Saeng;Ha, Sang-Chul;Jo, Jae-Sun
    • Korean Journal of Food Science and Technology
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    • v.31 no.4
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    • pp.945-951
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    • 1999
  • A simple and practical method for the determination of gardenia yellow in foods was developed. In this method, analysis of gardenia yellow in food products has been carried out by the detection of crocetin and/or geniposide as indicator compounds. As a new analytical method for gardenia yellow, we adopted crocetin, which is produced from colored components of gardenia yellow by alkaline hydrolysis, as an indicator compound. The analysis of gardenia yellow was performed by reverse phase high performance liquid chromatography using a Capcell pak $C_{18}$ column at wave length 240 nm (geniposide) and 435 nm (crocetin). The recovery rates of geniposide and crocetin were found to be 93.4% and 87.8% for Dan Mu Ji, 90.2% and 85.9% for milk, 92.8% and 86.5% for snack, respectively. With this method, the range of crocetin and geniposide contents $({\mu}g/g)$ were as follows: $ND{\sim}1.7$ and $ND{\sim}14.1$ for Dan Mu Ji, $ND{\sim}0.2$ and $ND{\sim}13.6$ for milk, $ND{\sim}1.6$ and $ND{\sim}0.9$ for snack, respectively. The detection limits of crocetin and geniposide were 0.07 ${\mu}g/g$ and 0.05 ${\mu}g/g$, respectively.

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Comparison and validation of rutin and quercetin contents according to the extraction method of tartary Buckwheat (Fagopyrum tataricum Gaertn.) (쓴메밀 종자의 추출방법에 따른 루틴 및 퀘세틴 함량 비교)

  • Kim, Su Jeong;Sohn, Hwang Bae;Kim, Geum Hee;Lee, Yu Young;Hong, Su Young;Kim, Ki Deog;Nam, Jeong Hwan;Chang, Dong Chil;Suh, Jong Taek;Koo, Bon Cheol;Kim, Yul Ho
    • Korean Journal of Food Science and Technology
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    • v.49 no.3
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    • pp.258-264
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    • 2017
  • The stability and accuracy of ultra-performance liquid chromatography (UPLC) used for evaluating the contents of rutin and quercetin in tartary buckwheat (Fagopyrum tataricum Gaertn.) seeds extracted by seven different extraction methods were determined. The seven extraction methods were reflux extraction (RE), ultra-sonification extraction (UE), stirrer extraction (SE), RE after UE (UE+RE), RE after SE (SE+RE), UE after SE (SE+UE), and RE with UE after SE (SE+UE+RE). Among the seven extraction methods used, RE yielded comparatively higher contents of rutin (2,277 mg/ 100 g) and quercetin (158 mg/100 g) than those yielded by other six extraction methods. The intra-day repeatability and inter-day precision of RE was 0.4-3.2% considering relative standard deviation (RSD), while accuracy was 88.8-102.4%. Therefore, RE with UPLC would be a rapid, accurate, and stable method for analyzing rutin and quercetin contents in tartary buckwheat.

A Case of the Shoulder-Hand Syndrome Caused by a Crush Injury of the Shoulder (견관절부 외상후 발생된 Shoulder-Hand Syndrome)

  • Jeon, Jae-Soo;Lee, Sung-Keun;Song, Hoo-Bin;Kim, Sun-Jong;Park, Wook;Kim, Sung-Yell
    • The Korean Journal of Pain
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    • v.2 no.2
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    • pp.155-166
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    • 1989
  • Bonica defined, that reflex sympathetic dystrophy (RSD) may develop pain, vasomotor abnoramalities, delayed functional recovery, and dystrophic changes on an affected area without major neurologic injury following trauma, surgery or one of several diseased states. This 45 year old male patient had been crushed on his left shoulder by a heavily laden rear car, during his job street cleaning about 10 years ago (1978). At first the pain was localizea only to the site of injury, but with time, it spreaded from the shoulder to the elbow and hand, with swelling. X-ray studies in the local clinic, showed no bone abnormalities of the affected site. During about 10 years following the injury, the had recieved several types of treatments such as nonsteroidal analgesics, steroid injections into the glenoidal cavity (10 times), physical therapy, some oriental herb medicines, and acupuncture over a period of 1~3 months annually. His shoulder pain and it's joint dysfunction persisted with recurrent paroxysmal aggrevation because of being mismanaged or neglected for a sufficiently long period these fore permiting progression of the sympathetic imbalance. On July 14 1988 when he visited our clinic. He complained of burning, aching and had a hyperpathic response or hyperesthesia in touch from the shoulder girdle to the elbow and the hand. Also the skin of the affected area was pale, cold, and there was much sweating of the axilla and palm, but no edema. The shoulder girdle was unable to move due to joint pain with marked weakness. We confirmed skin temperatures $5^{\circ}C$ lower than those of the unaffected axilla, elbow and palm of his hand, and his nails were slightly ridged with lateral arching and some were brittle. On X-ray findings of both the shoulder AP & lateral view, the left humerus and joint area showed diffuse post-traumatic osteoporosis and fibrous ankylozing with an osteoarthritis-like appearance. For evaluating the RSD and it's relief of pain, the left cervical sympathetic ganglion was blocked by injecting 0.5% bupivacaine 5 ml with normal saline 5 ml (=SGB). After 15 minutes following the SGB, the clinical efficacy of the block by the patients subjective score of pain intensity (=PSSPI), showed a 50% reduction of his shoulder and arm pain, which was burning in quality, and a hyperpathic response against palpation by the examiner. The skin temperatures of the axilla and palm rose to $4{\sim}5^{\circ}C$ more than those before the SGB. He felt that his left face and upper extremity became warmer than before the SGB, and that he had reduced sweating on his axilla and his palm. Horner's sign was also observed on his face and eyes. But his deep shoulder joint pain was not improved. For the control of the remaining shoulder joint pain, after 45 minutes following the SGB, a somatic sensory block was performed by injecting 0.5% bupivacaine 6 ml mixed with salmon calcitonin, $Tridol^{(R)}$, $Polydyn^{(R)}$ and triamcinolone into the fossa of the acromioclavicular joint region. The clinical effect of the somatic block showed an 80% releif of the deep joint pain by the PSSPI of the joint motion. Both blocks, as the above mentioned, were repeated a total of 28 times respectively, during 6 months, except the steroid was used just 3 times from the start. For maintaining the relieved pain level whilst using both blocks, we prescribed a low dose of clonazepam, prazocin, $Etravil^{(R)}$, codeine, etodolac micronized and antacids over 6 months. The result of the treatments were as follows; 1) The burning, aching and hyperpathic condition which accompanied with vaosmotor and pseudomotor dysfunction, disappeared gradually to almost nothing, within 3 weeks from the starting of the blocks every other day. 2) The joint disability of the affected area was improved little by little within 6 months. 3) The post-traumatic osteoporosis, fibrous ankylosis and marginal sclerosis with a narrowed joint, showed not much improvement on the X-ray findings (on April 25, 1989) 10 months later in the follow-up. 4) Now he has returned to his job as a street cleaner.

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