• Title/Summary/Keyword: LC/MSD

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Characteristics of Thiosulfinates and Volatile Sulfur Compounds from Blanched Garlic Reacted with Alliinase (Alliinase 첨가에 의한 열처리 마늘로부터 생성된 함황 화합물의 특성)

  • Choi, Yoon-Hee;Shim, You-Sin;Kim, Cheong-Tae;Lee, Chan;Shin, Dong-Bin
    • Korean Journal of Food Science and Technology
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    • v.39 no.6
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    • pp.600-607
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    • 2007
  • In this study, attempts were made to develop a method for controlling the volatile sulfur compounds in garlic. Crude alliinase extracted from fresh garlic was applied to garlic pulp blanched far 5 min at $100^{\circ}C$, and the changes in the thiosulfinates and volatile compounds of the blanched garlic pulp reacted with the enzyme were investigated. Eight kinds of thiosulfinates from garlic were separated by HPLC, and identified by LC/MS/MS. When the alliinase was added to the blanched garlic pulp at 100, 200, 300, or 400 units, and reacted for 15 min, respectively, thiosulfinates were generated in the amounts of 37, 68, 77, and 80% of the fresh garlic content (control). Under the same conditions, we analyzed the volatile compounds, where 28 peaks were identified by GC/MSD. Of the 28 peaks, 23 were volatile sulfur compounds. The results of the analysis showed that all the volatile compounds were generated at amounts of 25, 36, 66, and 76% of the content of the control, respectively. These results indicate that the sulfur compound content of garlic can be regulated, depending upon the reaction conditions of allinase.

Bioequivalence of EnalaceTM Tablet to RenitecTM Tablet (Enalapril maleate 10 mg) (레니텍® 정(말레인산 에날라프릴, 10 mg)에 대한 에나레이스 정의 생물학적 동등성)

  • Cho, Sung-Hee;Ha, Yong-Hwa;Hong, Sung-Je;Seo, Seong-Hoon;Rew, Jae-Hwan;Kim, Dong-Hyun;Lee, Kyung-Tae
    • Journal of Pharmaceutical Investigation
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    • v.33 no.3
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    • pp.229-235
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    • 2003
  • The purpose of the present study was to evaluate the bioequivalence of two enalapril maleate tablets, $Renitec^{TM}$ (MSD Korea Ltd.) and $Enalace^{TM}$ (Welfide Korea Ltd.), according to the guidelines of Korea Food and Drug Administration (KFDA). Twenty-four normal male volunteers, $22.33{\pm}2.55$ year in age and $66.54{\pm}8.30$ kg in body weight, were divided into two groups and a randomized $2{\times}2$ cross-over study was employed. After two tablets containing 10 mg of enalapril maleate per tablet were orally administered, blood was taken at predetermined time intervals and concentrations of enalapril in plasma were determined using LC-MS-MS. 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 $AUC_t,\;and\;C_{max}$ untransformed $T_{max}$. There were no sequence effects between two formulations in these parameters. The 90% confidence intervals for the log transformed data were acceptance range of log0.8 to log1.25$(e.g.,\;log1.02{\sim}log1.14\;and\;log1.03{\sim}log1.19\;for\;AUC_t\;and\;C_{max},\;respectively)$. The major parameters, $AUC_t,\;and\;C_{max}$, met the criteria of KDFA for bioequivalence indicating that $Enalace^{TM}$ tablet is bioequivalent to $Renitec^{TM}$ tablet.

Determination of residual pesticides in crude drugs - Gas chromatographic Analysis of 18 pesticides - (한약재중의 잔류농약 분석 - GC에 의한 18종 잔류농약의 분석 -)

  • Hwang, In-Sook;Choi, Byung-Hyun;Bae, Chong-Ho;Kim, Myung-Hee;Cho, Hae-Jeon
    • Korean Journal of Pharmacognosy
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    • v.32 no.3 s.126
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    • pp.200-211
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    • 2001
  • This study was carried out to determine the 11 organochlorine, 7 organophosphorus residual pesticides in 251 crude drugs. These residual pesticides in herbal drugs were extracted with acetonitrile and the extracts were cleaned up via LC-florisil solid phase extraction column. The prepared samples were assayed for pesticide residues using GC-ECD, NPD with capillary column and identified by GC-MSD. Recoveries were $63.9{\sim}111.5%$ in the organochlorine pesticides and $69.8{\sim}92.4%$ in the organophosphorus pesticides, and detection limits were $0.001{\sim}0.65\;ppm$ in the organochlorine pesticides and $0.0009{\sim}0.0074\;ppm$ in the organophosphorus pesticides. Pesticide residues were detected in 9 cases.

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Synthesis and pH-Dependent Micellization of a Novel Block Copolymer Containing s- Triazine Linkage

  • Pal Ravindra R.;Lee Doo Sung
    • Macromolecular Research
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    • v.13 no.5
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    • pp.373-384
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    • 2005
  • Novel pH-sensitive moieties containing an s-triazine ring were synthesized with sulfonamide and secondary amino groups. The synthesized pH-sensitive moieties were used for the synthesis of a pH-sensitive amphiphilic ABA triblock copolymer. The pH-sensitive triblock copolymer was composed of diblock copolymers, methoxy poly(ethylene glycol)-poly ($\varepsilon$-caprolactone-co-D,L-lactide) (MPEG-PCLA), and pH-sensitive moiety. These copolymers could be dissolved molecularly in both acidic and basic aqueous media at room temperature due to secondary amino and sulfonamide groups. The synthesized s-triazine rings containing pH-sensitive compounds were characterized by ${^1}H-NMR,\;{^13}C-NMR$, and LC/MSD spectral data. The synthesized diblock and triblock copolymers were also characterized by ${^1}H-NMR$ and GPC analyses. The critical micelle concentrations at various pH conditions were determined by fluorescence technique using pyrene as a probe. Furthermore, the micellization and demicellization study of the triblock copolymer was done with pH-sensitive groups. The sensitivity towards pH change was further established by acid-base titration.

Characteristics of Pesticide Residues in Leafy Vegetables Collected from Wholesale and Traditional Markets in Cheongju (청주지역 도매시장과 재래시장 유통 엽채류 중 농약의 잔류 특성)

  • Noh, Hyun-Ho;Lee, Kwang-Hun;Lee, Jae-Yun;Park, Hyo-Kyoung;Park, So-Hyun;Kim, Sun-Ho;Kyung, Kee-Sung
    • The Korean Journal of Pesticide Science
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    • v.15 no.4
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    • pp.453-462
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    • 2011
  • This study was carried out to survey the residual characteristics of pesticides and assess their safety. Nineteen agricultural commodities, collected from wholesale and traditional markets in Cheongju. Nineteen agricultural commodities including perilla leaves were collected from the markets on October 29th, 2010. Total 240 pesticides which can be analyzed by multiresidue analysis method by GLC and HPLC were monitored and the pesticides detected were confirmed by GC-MSD and LC-MS. Five pesticides, alachlor, bifenthrin, endosulfan, procymidone and triflumizole, were detected from five samples, such as welsh onion, leek and celery in case of wholesale market and perilla leaves and welsh onion in case of traditional market. Detection rate of 13.2% was obtained as a result of pesticide analysis but 2.6% of the pesticides detected exceeded their maximum residue limits. The estimated daily intakes (EDIs) and maximum permissible intakes (MPIs) of the pesticides detected were less than 26% and 0.05% of their acceptable daily intakes (ADIs) respectively, representing that residue levels of the pesticides detected would be safe.

Evaluation of the Bioequivalence of Simvastatin 20mg Tablets in Healthy Volunteers (조코 정에 대한 엘바스타 정의 생물학적 동등성 평가)

  • Yun, Hwi-yeol;Kang, Wonku;Kwon, Kwang-il
    • Korean Journal of Clinical Pharmacy
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    • v.15 no.1
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    • pp.41-45
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    • 2005
  • 심바스타틴은 cholesterol 생합성 과정에서 속도 조절 효소인 HMG-CoA reductase의 강력한 상경적 길항약으로서 고지혈증 치료에 널리 쓰이는 약물이다. 심바스타틴 제제인 MSD 사의 조코 20 mg정을 대조약으로 하여 시험약인 유영 제약의 엘바스타 20mg정의 생물학적 동등성 평가를 하기 위해 22명의 건강한 지원자를 모집하였다. 지원자를 두 군으로 나누어 2정씩 투여하였고 $2{\times}2$ 교차시험을 실시하였다. 심바스타틴의 혈장 중의 농도를 정량하기 위하여 발리데이션된 LC/MS/MS를 사용하였다. 채혈 시간은 투약 전 및 투약 후 0.5, 1, 1.5, 2, 2.5, 3, 4, 6, 8, 10, 12 시간에 걸쳐 총 12시점에 걸쳐 시행하였다. 생물학적 동등성을 판정하기 위한 파라미터로 12시간까지의 혈장 중 농도곡선 하 면적 ($AUC_{12hr}$)과 최고 혈중 농도($C_{max}$)를 사용하였다. 12시간 까지의 혈중 농도 곡선 하 면적의 기하 평균은 $17.30ng{\cdot}ml/hr$(시험약)과 $17.35ng{\cdot}ml/hr$(대조약)으로 나타났다. 최고 혈중 농도의 경우 각 각 5.08 ng/ml(시험약)과 5.20 ng/ml(대조약)으로 관찰 되었다. $AUC_{12hr}$의 경우 로그변환한 평균치 차의 $90{\%}$ 신뢰구간이 log0.8510 - log1.1694이었고, $C_{max}$의 경우 log0.8176 - log1.1649로 계산되어 두 항목 모두 log0.8-log1.25이어야 한다는 식품의약품 안전청과 FDA의 기준을 모두 만족시켰다. 이상의 결과를 종합하면 시험약 엘바스타 정 20mg은 대조약 조코정 20 mg에 대하여 생물학적 동등한 것으로 판정되었다.트리머 전기비저항 탐사를 수행하였다. 이를 통해 하저에 케이블을 설치하는 방식에 비해 매우 신속하고 경제적으로 하저에 분포하는 이상대의 분포범위와 발달방향을 규명할 수 있었다.대에 대해 가장 효과적이다. 모델과 현장 적용 결과들을 통해 GRM SSM 방법을 이용하여 불규칙한 굴절면을 가진 지층들에 대해 좀 더 신뢰할 수 있는 정밀한 탄성파 속도를 산출할 수 있음을 보여주고 있다.별한 주의를 기울여야 한다.EX>$\alpha/\beta$=10인 경우 $62.0\~121.9\;Gy_{10}$ (중앙값: $93.0\;Gy_{10}$)의 분포를, ${\alpha/\beta}=3$인 경우 $93.6\~187.3\;Gy_3$ (중앙값=$137.6\;Gy_3$ )의 분포를 보였다. MD-BED $Gy_3$는 직장합병증 발생과의 관계는 통계적으로 유의하였고, 방광합병증과는 유의하지 않았다. 직장합병증과의 연관성은 MD-BED $Gy_3$보다 개별 환자의 직장전벽 총 선량 BED값인 R-BED $Gy_3$가 훨씬 더 높았다. 요도카테터 풍선의 후방지점이 대변하는 방광의 총 선량 BED값인 V-BED $Gy_3$도 방광합병증과 경향성 테스트에서 통계적 유의성을 보였다. 하지만, 어떠한 방사선선량도 골반제어율과 의미 있는 상관관계를 보이지 않았다. 본 기관에서 주치의의 선호도에 따라 강내근접치료가 외부방사선치료의 중간에 시행되는 형태인 샌드위치기법과 외부방사선치료 후반부에 시행되는 순차적 기법으로 구분하였을 때, 두 방식간 치료성적 및 합병증의 차이는 없었다. 총 치료기간에 대한 분석에서는 치료기간이 길어질수록 재발 위험이 커지는 경향을 보였으나, 나이 및 병기, 종양의 크기, MD-BED $Gy_{10}$

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Bioequivalence of LosartanTM Tablet to CozzarTM Tablet (Losartan Kalium 50 mg) (코자 정(로자탄 칼륨 50 mg)에 대한 로자르탄 정의 생물학적동등성)

  • Kim, Yong-Won;Park, Wan-Su;Kim, Sung-Su;Seo, Ji-Hyung;Cho, Sung-Hee;Lee, Heon-Woo;Rew, Jae-Hwan;Lee, Kyung-Tae
    • Journal of Pharmaceutical Investigation
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    • v.36 no.2
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    • pp.131-136
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    • 2006
  • The purpose of the present study was to evaluate the bioequivalence of two losartan tablets, $Cozaar^{TM}$ tablet (MSD Korea. Co., Ltd., Seoul, Korea, reference drug) and $Losartan^{TM}$ tablet (DaeWon Pharm. Co., Ltd., Korea, test drug), according to the guidelines of Korea Food and Drug Administration (KFDA). Twenty-four healthy male Korean volunteers received two tablets at the losartan kalium dose of 100 mg in a $2\;{\time}\;2$ crossover study. There was a one-week washout period between the doses. Plasma concentrations of losartan were monitored by an LC-MS/MS for over a period of 12 hr after the administration. $AUC_t$ (the area under the plasma concentration-time curve from time zero to 12 hr) was calculated by the linear trapezoidal rule method. $C_{max}$ (maximum plasma drug concentration) and $T_{max}$ (time to reach $C_{max}$) were compiled from the plasma concentration-time data. Analysis of variance was carried out using logarithmically transformed $AUC_t$ and $C_{max}$. No significant sequence effect was found for all of the bioavailability parameters indicating that the crossover design was properly performed. The 90% confidence intervals of the $AUC_t$ ratio and the $C_{max}$ ratio for $Cozaar^{TM}/Losartan^{TM}$ were $log\;0.97{\sim}log\;1.12\;and\;log\;0.93{\sim}log\;1.23$, respectively. These values were within the acceptable bioequivalence intervals of $log\;0.80{\sim}log\;1.25$. Taken together, our study demonstrated the bioequivalence of $Cozaar^{TM}$ and $Losartan^TM$ with respect to the rate and extent of absorption.

Establishment of the Korean total diet study (TDS) model in consideration to pesticide intake (한국형 총식이섭취조사(Total Diet Study, TDS) 모델 확립을 위한 농약섭취수준에 대한 접근)

  • Yang, An-Gel;Shim, Ki-Hoon;Choi, Ok-Ja;Park, Jong-Hyouk;Do, Jung-Ah;Oh, Jae-Ho;Hwang, In Gyun;Shim, Jae-Han
    • The Korean Journal of Pesticide Science
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    • v.16 no.2
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    • pp.151-162
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    • 2012
  • This study was carried out to establish Korean total diet study (TDS) model for estimating pesticide residue in food samples. In addition, pesticide residues of food samples were monitored by setting the standards of established Korean total diet study model. For monitoring, first step were selection of total 102 species food samples, second step were selection of total 70 species food samples, and third step were selection of total 12 representative diet and 109 species food samples. Ninety-eight pesticides were analyzed using $GC-{\mu}ECD$, GC-MS, and LC-MS/MS after QuEChERS sample preparation method. The residue levels in detected food samples were below the maximum residue limit (MRL). Establishment of the Korean total diet study model means providing safe food for consumers, secure the safety of food samples and provide ongoing information to agricultural producers about use of pesticides.

Monitoring and Safety Assessment of Pesticide Residues on Agricultural Products Sold via Online Websites (온라인 판매 농산물 잔류농약 실태 및 안전성 평가)

  • Park, Duck Woong;Kim, Ae Gyeong;Kim, Tae Sun;Yang, Yong Shik;Kim, Gwang Gon;Chang, Gil Sik;Ha, Dong Ryong;Kim, Eun Sun;Cho, Bae Sik
    • The Korean Journal of Pesticide Science
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    • v.19 no.1
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    • pp.22-31
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    • 2015
  • This study was carried out to monitor the current status of pesticide residues in selling agricultural products via online and assessed their safety in 2014. A total of 124 samples were purchased six times from March to August 2014 twenty online shopping malls randomly. These samples were analysed 208 pesticides by multiresidue method using a GC-ECD/NPD and a LC-MS/MS and confirmed by a GC-MSD. As a result of analysis, residual pesticides samples were 11 (8.9%) such as leek, young radish, welsh onion etc, of which 2 samples (1.6%) such as sesame bud (Chlorothalonil), artemisia (Chlorpyrifos) were violated Korea Maximum Residue limits (MRLs). 11 kinds of pesticides (19 times) were detected in 11 samples. Risk assessment evaluated human health exposure with the ratio of EDI (Estimated daily intake) to ADI (Acceptable daily intake) of pesticides detected. %ADI (the ratios of EDI to ADI) were 0.04~95.70% and some samples represented a fairly dangerous levels. In particular, Chlorothalonil in the sesame bud was shown as a significant risk close to 100% of %ADI. Accordingly, it is recommended to strengthen a safety check on agricultural products in online sales.

A Survey on Pesticide Residues of Commercial Flowering Teas (국내 유통중인 식용꽃차의 잔류농약 실태조사)

  • Park, Jungwook;Lee, Hyanghee;Oh, Musul;Kim, Jongpil;Jang, Taekwan;You, Youna;Ha, Dongryong;Kim, Eunsun;Seo, Kyewon
    • The Korean Journal of Pesticide Science
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    • v.17 no.1
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    • pp.1-5
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    • 2013
  • This study was conducted to the amount of pesticide residue in 21 different kinds of 100 commercial flowering teas. Multi-residue analyses of 203 pesticides was performed using the GC-ECD, GC-NPD, GC-MSD, and LC-MS/MS. Pesticide residues were detected in 4 samples (4%) of which 4 samples (4%) violated the maximum residue limits. 4 samples violating the limit were all imported teas. Pesticides detected were chlorpyrifos, flufenoxuron, lufenuron, pyrimethanil and methoxyfenozide. These results indicate the need of continuous monitoring of pesticide residue needs for safety of flowering teas.