• Title/Summary/Keyword: HPLC detector

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Establishment of Pre-Harvest Residue Limit for Pyrimethanil and Methoxyfenozide during Cultivation of grape (포도(Vitis vinifera L.) 중 Pyrimethanil 및 Methoxyfenozide의 생산단계 잔류허용기준 설정)

  • Kim, Ji Yoon;Woo, Min Ji;Hur, Kyung Jin;Manoharan, Saravanan;Kwon, Chan-Hyeok;Hur, Jang Hyun
    • The Korean Journal of Pesticide Science
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    • v.19 no.2
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    • pp.81-87
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    • 2015
  • The present study was aimed to predict the pre-harvest residue limits (PHRLs) of pyrimethanil (fungicide) and methoxyfenozide (insecticide) in grape, and to estimate their biological half-lives and residual characteristics. The pesticides were sprayed once on grape in two different fields 10 days before harvest. At the end of 0, 1, 2, 3, 5, 7 and 10 days after application, samples were harvested for further analysis. The residual pesticides were extracted with acetonitrile and partitioned with dichloromethane, and the high-performance liquid chromatography with diode array detector (HPLC/DAD) was employed for the residue analysis. The results obtained in the present study show that the limit of detection of both pesticides were found to be $0.01mg\;kg^{-1}$. The recoveries of these pesticides were ranged between 80.6% and 102.5% with coefficient of variation lower than 10%. The biological half-lives of both pesticides were observed in field 1 and field 2 which shows 7.7 and 7.4 days for pyrimethanil and 5.1 and 6.1 days for methoxyfenozide, respectively. Further, the PHRL of pyrimethanil and methoxyfenozide was found to be $8.90mg\;kg^{-1}$ and $5.51mg\;kg^{-1}$, respectively at 10 days before harvest. Consequently, the present study suggests that the residual amounts of both pesticides will be lower than the maximum residue limits (MRLs) when grape is harvested.

Bioequivalence of Burophil Capsule to Surfolase Capsule (Acebrophylline 100 mg) (설포라제 캡슐(아세브로필린 100 mg)에 대한 부로필 캡슐의 생물학적 동등성)

  • Cho, Hea-Young;Park, Eun-Ja;Kang, Hyun-Ah;Kim, Se-Mi;Park, Chan-Ho;Oh, In-Joon;Lim, Dong-Koo;Lee, Myung-Hee;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.35 no.3
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    • pp.179-185
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    • 2005
  • Acebrophylline is a compound produced by salifying ambroxol with theophylline-7 -acetic acid. After acebrophylline administration, the salt splits into these two components which feature a peculiar pharmacokinetic behavior, an adequate ambroxol and a low theophylline-7-acetic acid serum levels. The purpose of the present study was to evaluate the bioequivalence of two acebrophylline capsules, Surfolase (Hyundai Pharm. lnd. Co., Ltd.) and Burophil (Kuhnil Pharm. Co., Ltd.), according to the guidelines of the Korea Food and Drug Administration (KFDA). The release of ambroxol from the two acebrophylline formulations in vitro was tested using KP VIII Apparatus II method with various dissolution media (pH 1.2, 4.0, 6.8 buffer solution and water). Twenty eight healthy male subjects, $23.25{\pm}1.43$ years in age and $64.82{\pm}6.77$ kg in body weight, were divided into two groups and a randomized $2{\times}2$ cross-over study was employed. After two capsules containing 100 mg as acebrophylline were orally administered, blood was taken at predetermined time intervals and the concentrations of ambroxol in serum were determined using HPLC with electrochemical detector (ECD). The dissolution profiles of two formulations were similar at all dissolution media. In addition, the pharmacokinetic parameters such as $AUC_t$, $C_{max}$ and $T_{max}$ were calculated and ANOVA test was utilized for the statistical analysis of the parameters using logarithmically transformed $AUC_t$, $C_{max}$ and untransformed $T_{max}$. The results showed that the differences between two formulations based on the reference drug Surfolase, were -1.64, -3.33 and -0.92% for $AUC_t$, $C_{max}$ and $T_{max}$, respectively. There were no sequence effects between two formulations in these parameters. The 90% confidence intervals using logarithmically transformed data were within the acceptance range of log 0.8 to log 1.25 $(e.g., \;log\;0.93{\sim}log\;1.05\;and\;log\;0.88{\sim}log\;1.05$ for $AUC_t$, and $C_{max}$, respectively). Thus, the criteria of the KFDA bioequivalence guideline were satisfied, indicating Burophil capsule was bioequivalent to Surfolase capsule.

Bioequivalence of SCD Zaltoprofen Tablet to Soleton® Tablet (Zaltoprofen 80 mg) (솔레톤 정(잘토프로펜 80 mg)에 대한 삼천당잘토프로펜 정의 생물학적동등성)

  • Kang, Hyun-Ah;Park, Sun-Ae;Kim, Dong-Ho;Kim, Hwan-Ho;Yun, Hwa;Kim, Kyng-Ran;Yoo, Hee-Doo;Park, Eun-Ja;Cho, Hye-Young;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.36 no.3
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    • pp.209-215
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    • 2006
  • Zaltoprofen, (2-(10,11-dihydro-10-oxodibenzo[b,f]thiepin-2-yl)propionic acid) is an NSAID with powerful anti-inflammatory effects as well as an analgesic action on inflammatory pain. The purpose of the present study was to evaluate the bioequivalence of two zaltoprofen tablets, $Soleton^{\circledR}$ (CJ Corp.) and SCD Zaltoprofen (Samchundang Pharmaceutical Co., Ltd.), according to the guidelines of the Korea Food and Drug Administration (KFDA). The release of zaltoprofen from the two zatoprofen formulations in vitro was tested using KP Vlll Apparatus ll method with various dissolution media. Twenty six healthy male subjects, $23.2{\pm}2.26$ years in age and$64.7{\pm}8.08$ kg in body weight, were divided into two groups and a randomized $2{\times}2$ cross-over study was employed. After a single tablet containing 80 mg as zaltoprofen was orally administered, blood samples were taken at predetermined time intervals and the concentrations of zaltoprofen in serum were determined using HPLC with UV detector. The dissolution profiles of two formulations were similar in all tested dissolution media. The pharmacokinetic parameters such as $AUC_t$, $C_{max}$ and $T_{max}$ were calculated, and ANOVA test was utilized for the statistical analysis of the parameters using logarithmically transformed $AUC_t$, $C_{max}$ and untransformed $T_{max}$. The results showed that the differences between two formulations based on the reference drug, $Soleton^{\circledR}$ were 6.33, 5.91 and 17.7% for $AUC_t$, $C_{max}$ and untransformed $T_{max}$, respectively. There were no sequence effects between two formulations in these parameters. The 90% confidence intervals using logarithmically transformed data were within the acceptance range of log 0.8 to log 1.25 (e.g.,log $1.01{\sim}1og\;1.11$ and log $0.928{\sim}1og\;1.18$ for $AUC_t$ and $C_{max}$, respectively). Thus, the criteria of the KFDA bioequivalence guideline were satisfied, indicating SCD Zaltoprofen tablet was bioequivalent to $Soleton^{\circledR}$ tablet.

Analytical method of aflatoxins in edible oil and infant-children foods (식용유지와 영유아식품 중 아플라톡신 분석방법)

  • Hu, Soo-Jung;Park, Seung-Young;Kim, Soon-Sun;Lee, Joon-Goo;Song, Ji-Young;Kang, Eun-Gi;Lee, Hyun-Sook;Cho, Dae-Hyun
    • Analytical Science and Technology
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    • v.24 no.2
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    • pp.150-157
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    • 2011
  • Aflatoxins are secondary metabolites of the molds of Aspergillus flavus and Aspergillus parasiticus. They are highly carcinogenic compounds and can affect a wide range of vegetable commodities such as cereals (especially corn), nuts, peanuts, fruits and oil seeds, in the field and during storage. In fact, oilseeds are often stored for weeks in conditions that promote the mould growth, and the possible consequent presence of aflatoxins in oilseeds can lead to their transfer in oil. In addition, aflatoxins can be found as a natural contaminant in multi-cereals and beans making baby food for infants and young-children. The objective of this study was to validate the liquid extraction method or develop an analytical method for edible oil and infant-children foods. Therefore, this study developed condition of extract for aflatoxins ($B_1$, $B_2$, $G_1$ and $G_2$) in edible oil using a high performance liquid chromatography with florescence detector (HPLC/FLD). Aflatoxins were extracted from edible oil samples by means of MSPD (Matrix solid phased dispersion), utilizing $C_{18}$ as dispersing material and purified by using immunoaffinity column. The gression line coefficients were above 0.999. The recoveries for aflatoxins ranged from 85.9 to 93.0%, and relative standard deviations were below 5.7%. The new developed method of aflatoxins effectively enhanced recoveries by using MSPD-Immunoaffinity column compared with liquid extraction. The analytical method for liquid extraction of aflatoxin was appropriate for infant-children food. Reviewing the current method, the recoveries of aflatoxins ($B_1$, $B_2$, $G_1$ and $G_2$) were 89.5~92.3%.

Varietal Analysis and Quantification of Resveratrol in Mulberry Fruits (뽕나무 계통별 오디의 레스베라트롤 함량 분석)

  • Kim Hyun-Bok;Kim Jung-Bong;Kim Sun-Lim
    • Journal of Sericultural and Entomological Science
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    • v.47 no.2
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    • pp.51-55
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    • 2005
  • Resveratrol is naturally occurring phytoalexin compounds produced by grape berries, peanuts, and their products in response to stress such as fungal infection, heavy metal ions or UV irradiation. The objective of this study was to develope a reliable high performance liquid chromatographic (HPLC) method for the quantitative determination of trans-resveratrol in mulberry fruit. Samples were extracted in 80% MeOH and filtered with $0.45{\mu}m$ syringe filter. The transresveratrol was separated Waters $C_{18}$ column, using a mobile phase containing 0.025% trifluroacetic acid in 5% acetonitril and 0.035% trifluroacetic acid in 50% acetonitril, detected by photodiode array detector (PDA) at 254 nm and the flow rate was 1ml/min. Under this analytical condition, the mean content of mulberry fruits (fifty varieties) was $777.3{\pm}585.9ppm$. Among the tested samples, 'Mansaengbaekpinosang (II)' was the highest level in 3450.6 ppm. However four accessions including 'Gukbu', 'Sabangso (I)', 'Simseol' and yield mulberry fruit were not able to detected. Eight suitable varieties selected for the production of fruit were 'Jeolgokchosaeng (Chungbuk)' 777.8 ppm, 'Dangsang 7' 771.1 ppm, 'Jangsosang' 133.9 ppm, 'Susungppong' 31.1 ppm, 'Suwonnosang' 639.7 ppm, 'Palcheongsipyung' 1475.9 ppm, 'Kangsun' 864.0 ppm, and 'Jukcheonchosaeng' 1458.5 ppm. 'Daesungppong' which was the first authorized variety for the production of mulberry fruit was 1236.7 ppm. In conclusion, these results suggest that mulberry including fruit and leaf may a good new resource for resveratrol production.

Sugar and Sodium Content of Franchise Chickens and Market Chickens (프랜차이즈 치킨과 대형마트 내 판매 치킨의 당과 나트륨 함량 조사)

  • Lee, Young-Ju;Jung, So-Young;Kim, Nam-Hoon;Park, Young-Ae;Jo, Ju-Yeon;Kim, Youn-Cheon;Lee, Sang-Me;Kim, Moo-Sang
    • Journal of Food Hygiene and Safety
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    • v.35 no.2
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    • pp.118-124
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    • 2020
  • We investigated the content of sugar and sodium in 4 types of chicken (fried, seasoned, soy sauce-flavored, cheese powder-flavored). A total of 123 samples were collected from franchise stores and markets in Seoul. The sugar content of chicken samples was analyzed by HPLC-ELSD (High Performance Liquid Chromatography-Evaporative Light Scattering Detector). The average sugar content of seasoned chicken was highest at 8.7±2.3 g/100 g while that of fried chicken was lowest at 0.6±0.3 g/100 g. The average content of sugar sorted by place of sale showed a significant difference (P<0.05). The sodium content in chicken samples was analysed using the ICP-OES (Inductively Coupled Plasma-Optical Emission Spectrometry). The sodium content of seasoned chicken with cheese powder was the highest at 627.0±109.2 mg/100 g and that of fried chicken was the lowest at 448.0±65.3 mg/100 g. The sugar content of seasoned chicken sold in both franchise stores and markets was found to exceed the 50 g daily level as recommended by the WHO. In addition, the average sodium content in seasoned chicken (franchise stores and markets) and cheese-powdered chicken was more than twice as high as the daily 2,000 mg recommended by the WHO.

Bioequivalence of Carvelol Tablet to Dilatrend Tablet (Carvedilol 25 mg) (딜라트렌 정(카르베딜롤 25 mg)에 대한 카베롤 정의 생물학적 동등성)

  • Cho, Hea-Young;Lee, Moon-Seok;Park, Soon-Cheol;Lim, Dong-Koo;Moon, Jai-Dong;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.31 no.4
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    • pp.289-295
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    • 2001
  • Carvedilol is an antihypertensive and antianginal compound that combines nonselective beta-adrenoceptor blocking and vasodilation properties and is devoid of intrinsic sympathomimetic activity. The purpose of the present study was to evaluate the bioequivalence of two carvedilol tablets, $Dilatrend^{TM}$ (Chong Kun Dang Pharmaceutical Co., Ltd.) and $Carvelol^{TM}$ (Dae Won Pharmaceutical Co., Ltd.), according to the prior and revised guidelines of Korea Food and Drug Administration (KFDA). The carvedilol release from the two carvedilol tablets in vitro was tested using KP VII Apparatus II method with various different kinds of dissolution media (pH 1.2, 4.0, 6.8 buffer solution, water and blend of PSB80 into water). Eighteen normal male volunteers, $24.22{\pm}1.86$ years in age and $64.81{\pm}4.56\;kg$ in body weight, were divided into two groups and a randomized $2{\times}2$ cross-over study was employed. After one tablet containing 25 mg of carvedilol was orally administered, blood was taken at predetermined time intervals and the concentrations of carvedilol in serum were determined using HPLC method with fluorescence detector. The dissolution profiles of two carvedilol tablets were very similar at all dissolution media. Besides, the pharmacokinetic parameters such as $AUC_t$, $C_{max}$ and $T_{max}$ were calculated and ANOVA test was utilized for the statistical analysis of the parameters using non-transformed and logarithmically transformed $AUC_t$ and $C_{max}$. The results showed that the differences in $AUC_t$, $C_{max}$ and $T_{max}$ between two tablets based on the $Dilatrend^{TM}$ were 2.23%, -2.00% and 0.00%, respectively. Minimum detectable differences $({\Delta})$ at ${\alpha}=0.05$ and $1-{\beta}=0.8$ were less than 20% (e.g., 13.55% and 17.61% for $AUC_t$ and $C_{max}$, respectively). The powers $(l-{\beta})$ at ${\alpha}=0.05$, ${\Delta}=0.2$ for $AUC_t$ and $C_{max}$ were 98.08% and 88.81%, respectively. The 90% confidence intervals were within ${\pm}20%$ (e.g., $-5.69{\sim}10.16$ and $-12.30{\sim}8.30$ for $AUC_t$ and $C_{max}$, respectively). There were no sequence effect between two tablets in logarithmically transformed $AUC_t$ and $C_{max}$. The 90% confidence intervals using logarithmically transformed were within the acceptance range of log(0.8) to log(1.25) (e.g., $0.95{\sim}1.11$ and $0.89{\sim}1.09$ for $AUC_t$ and $C_{max}$, respectively). Two parameters met the criteria of prior and revised KFDA guideline for bioequivalence, indicating that $Carvelol^{TM}$ tablet is bioequivalent to $Dilatrend^{TM}$ tablet.

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Total Sugar and Artificial Sweetener Contents of Health Functional Foods in Seoul (서울지역 유통 건강기능식품의 당 및 인공감미료 함량)

  • Cho, In-soon;Cho, Tae-hee;Lee, Jae-kyoo;Lee, Yun-jeoung;Kim, Si-jung;Choi, Hee-jin;Shin, Ki-young;Oh, Young-hee
    • Journal of Food Hygiene and Safety
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    • v.32 no.4
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    • pp.314-320
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    • 2017
  • This study was carried out to investigate and evaluate total sugar and artificial sweetener contents in health functional foods. In this study, HPLC with evaporative light scattering detector (ELSD) and HPLC-UV were used to determine the contents of total sugar and artificial sweetener in health functional foods. Sixty-six chewable products and sixty red ginseng products were collected from markets in Seoul. The average content of 126 samples per daily intake portion was 1.96 g ranging from not-detected (N.D.) to 12.61 g. The mean total sugar content per serving of chewable product was 1.26 g and N.D. to 10.39 g. The average amount of total sugar per daily intake of ginseng and red ginseng was 2.70 g and N.D. to 12.61 g. The average amount of sugar per daily intake of chewable products was 2.10 g for children, 1.43 g for nutrients, and 0.35 g for functional raw material. For children's products, the content of sugar per serving was ranged from 1.03 g to 5.33 g, from N.D. to 10.39 g for nutrients and from N.D. to 2.61 g for functional raw materials. The average content of sugar per daily intake of ginseng and red ginseng product was 4.25 g in liquid product, 1.51 g in concentrate product and 1.49 g in powder product. The contents of sugar per the daily intake of the liquid product ranged from N.D. to 10.80 g, from 0.01 g to 12.61 g for the concentrated product, and from 0.06 g to 5.64 g for the powdered product. Analysis of artificial sweeteners showed that artificial sweeteners were detected in three cases. No artificial sweeteners were detected in ginseng and red ginseng products. Two of the chewable products and one of the functional raw materials were detected. The detected artificial sweeteners were aspartame, 3.09 g/kg in nutrients and 1.09 g/kg in functional raw material.

Comparision of Preparation Methods for Water Soluble Vitamin Analysis in Foods by Reversed-Phase High Performance Liquid Chromatography (역상 고속 액체 크로마토그래피에 의한 식품 중 수용성 비타민 분석을 위한 전처리법의 비교)

  • Kim, Hyung-Soo;Jang, Duck-Kyu;Woo, Dong-Kyun;Woo, Kang-Lyung
    • Korean Journal of Food Science and Technology
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    • v.34 no.2
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    • pp.141-150
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    • 2002
  • Owing to a need for simple extraction and purification for analysis of water soluble vitamins in food samples by RP-HPLC with UV-detector, the methods of bromelain and protease hydrolysis and $C_{18}$ Sep-Pak solid phase extraction were employed. The recoveries of standard water soluble vitamins by the bromelain and protease hydrolysis and $C_{18}$ Sep-Pak solid phase extraction were significantly high compared to AOAC methods in most of vitamins. The contents of pyridoxal determined with protest in the pork was similar, but in the bromelain hydrolysis and AOAC method, was high compared to the results of reference. The niacinamide, thiamin and riboflavin determined with bromelain and protease hydrolysis showed similar values to the results of references. In the potato, pyridoxamine was detected in the AOAC method, which was not detected in the bromelain and protease hydrolysis methods. Pyridoxal contents in the protease hydrolysis and AOAC methods were very similar to the results of references. The recoveries of fortified standard vitamins in food samples were significantly high and accurate compared to those of AOAC methods. The extraction and purification with $C_{18}$ Sep-Pak solid extractor might be considered superior method for the determination of water soluble vitamins in food samples.

Development of Analysis Method of Caffeine and Content Survey in Commercial Foods by HPLC (HPLC를 이용한 카페인의 분석법 개발 및 시판 식품중 함유량 조사)

  • Kim, Hee-Yun;Lee, Young-Ja;Hong, Ki-Hyoung;Lee, Chul-Won;Kim, Kil-Saeng;Ha, Sang-Chul
    • Korean Journal of Food Science and Technology
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    • v.31 no.6
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    • pp.1471-1476
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    • 1999
  • A simple and practical method for determination of caffeine in foods was developed. The analysis of caffeine was performed by reverse phase high performance liquid chromatography using a ${\mu}-Bondapak\;C_{18}$ column at isocratic condition with methanol-acetic acid-water(20 : 1 : 79) on UV detector at 280 nm. The clean-up and extraction of caffeine in samples were based on a simple pretreatment using a Sep-Pak $C_{18}$ cartridge. Recovery rates obtained with this method for cider, candy, cookie, milk, ice cream and persimmon leaf tea were 99.23%, 99.50%, 99.17%, 99.37%, 98.93% and 99.10% respectively. And the detection limit of caffeine was $0.1\;{\mu}g/mL$. With this method, the range of caffeine contents extracted from coffee, green tea, black tea, Oolong tea(tea bag), soft drinks, ice cream, milk and commercial confectionery were $3.38{\sim}37.50\;mg/g,\;16.30{\sim}26.10\;mg/g,\;10.80{\sim}16.65\;mg/g,\;11.25\;mg/g,\;0.06{\sim}0.11\;mg/g,\;0.04{\sim}0.44\;mg/g,\;0.04{\sim}0.39\;mg/g\;and\;0.10{\sim}1.80\;mg/g$, respectively. But caffeine was not detected in the other tea such as Acanthopanax sessiliflorum tea, Angelica gigas tea, Angelica tea, Arrow root tea, Duchu'ng tea, Dunggulle tea, Ganoerma lucidum tea, Ginger tea powder, Persimmon leaf tea, Ssanghwa tea and Cocoa mix powder.

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