• 제목/요약/키워드: reversed phase

검색결과 605건 처리시간 0.023초

사무직 근로자들의 VDT 증후군 예방을 위한 자동 관찰 및 진동 피드백 시스템의 효과성 검증 (The Effect of Automated Observation and Vibration Feedback System for Preventing VDT Syndrome of Office Workers)

  • 안지연;오세진
    • 한국안전학회지
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    • 제34권3호
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    • pp.75-82
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    • 2019
  • The purpose of this study was to evaluate the effectiveness of a vibration feedback system in improving two safe seating postures of office workers. In addition, the relative effectiveness of positive and negative feedback procedures was examined. Participants were four office workers. The dependent variables were the percentages of time participants spent in the safe sitting postures including shoulder, back, and overall body positions during the experimental sessions. A multiple-baseline design counterbalanced across participants was adopted. For two participants, the negative procedure was introduced first after baseline and positive procedure was introduced in the next phase. For the other two participants, the sequence of introducing the positive and negative feedback procedures was reversed. The result showed that the vibration feedback system, regardless of the type of the procedure, was effective in improving the safe sitting postures for all participants. However, the difference between the two procedures was not clearly shown. The benefits of the automated observation and vibration feedback system in workers' safety were discussed.

참깨 종실의 항산화 성분 정량분석 연구 (Quantitative Analysis of Antioxidants in Sesame Seed)

  • 류수노;이정일;강삼식;최원열
    • 한국작물학회지
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    • 제37권4호
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    • pp.377-382
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    • 1992
  • 본 연구는 고항산화 양질 육종의 체계확립을 위해서 참깨에 있는 특수성분인 sesamin, sesamolin의 표준물질을 동정하고 그 분석기술을 개발하였는바 그 결과는 다음과 같다. 1. 한국산 참깨로부터 sesamin, sesamolin 성분을 분리하여 화학적 구조를 분광학적 방법(UV, $^1$H와 $^{13}$C-NMR, MS)으로 확인하여 sesamin, sesamolin의 표준물질을 동정하였다. 2. 참깨 lignan성분의 추출 및 분리에는 Unsaponifiable fration 보다 MeOH 냉온처리가 더 효과적이었다. 3. 검량선의 회귀직선의 방정식은 sesamin에서 y=53924.43+1277.93x(r=0.9993)이었고 sesamolin의 경우는 y=11034.95+1188.38x(r=0.9994)로 추정되었다. 4. 한국산 참깨의 lignan 성분함량은 단백깨의 경우 sesamin 0.42% sesamolin 0.3%로 나타났다.

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Optimization of Ceramide Analysis Method Using LC-MS in Cosmetics

  • Su-Jin Park;Hee-Jin Yoo;Duck-Hyun Kim;Ji-Won Park;Eunji Jeon;Abhik Mojumdar;Kun Cho
    • Mass Spectrometry Letters
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    • 제15권1호
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    • pp.49-53
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    • 2024
  • Ceramide is a lipid in which sphingoid bases and fatty acids are linked by amide bonds. As a marker of skin disease in the human stratum corneum, its disease-causing and therapeutic effects have been partially confirmed, and it is therefore an important element in commercially available cosmetic formulations. However, structural diversity caused by differences in the chain length, number, and location of hydroxyl groups makes quality control difficult. In this study, a method was established to separate different ceramide species using reversed-phase LC-MS/MS and thus enable qualitative evaluation. Separation of four standards was achieved within a short retention time, and the accuracy and sensitivity of the method were demonstrated by the low limit of detection (LOD) calculated based on the calibration curve showing linearity, with R2 > 0.994. After verification of reproducibility and reliability through intra- and inter-day analyses, the efficiency of the method was confirmed through analysis of commercial cosmetic raw materials.

글리피짓 체내동태 연구를 위한 혈청 중 글리피짓의 HPLC 정량법 검증 (Validation of an HPLC Method for the Pharmacokinetic Study of Glipizide in Human)

  • 조혜영;이화정;최후균;이용복
    • Journal of Pharmaceutical Investigation
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    • 제35권3호
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    • pp.137-142
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    • 2005
  • A rapid, selective and sensitive reversed-phase HPLC method for the determination of glipizide in human serum was validated and applied to the pharmacokinetic study of glipizide. Glipizide and internal standard, tolbutamide, were extracted from human serum by liquid-liquid extraction with benzene and analyzed on a Nova Pak $C_{18}\;60{\AA}$ column with the mobile phase of acetonitrile-potassium dihydrogen phosphate (10 mM, pH 3.5) (4:6, v/v). Detection wavelength of 275 nm and flow rate of 0.7 ml/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^3$ factorial design using a fixed glipizide concentration (500 ng/ ml) with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 10-1000 ng/ml with correlation coefficient greater than 0.999. The lower limit of quantitation using 0.5 ml of serum was 10.0 ng/ml, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the quality control samples ranged from 82.6 to 105.0% for glipizide with overall precision (% C.V.) being 1.13-13.20%. The percent recovery for human serum was in the range of 85.2 93.5%. Stability studies showed that glipizide was stable during storage, or during the assay procedure in human serum. The peak area and retention time of glipizide were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of glipizide in human serum samples for the pharmacokinetic studies at three different laboratories, demonstrating the suitability of the method.

테르페나딘 체내동태 연구를 위한 혈청 중 펙소페나딘의 HPLC 정량법 개발 및 검증 (Development and Validation of an HPLC Method for the Pharmacokinetic Study of Fexofenadine in Human)

  • 조혜영;강현아;김윤균;최후균;이용복
    • Journal of Pharmaceutical Investigation
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    • 제35권6호
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    • pp.437-443
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    • 2005
  • A rapid, selective and sensitive reversed-phase HPLC method for the determination of a major metabolite of terfenadine, fexofenadine, in human serum was developed, validated, and applied to the pharmacokinetic study of terfenadine. Fexofenadine and internal standard, haloperidol were extracted from human serum by liquid-liquid extraction with acetonitrile and analyzed on a $Symmetry^{TM}$ C8 column with the mobile phase of 1% triethylamine phosphate (pH 3.7)-acetonitrile (67:33, v/v, adjusted to pH 5.6 with triethylamine). Detection wavelength of 230 nm for excitation, 280 nm for emission and flow rate of 1.0 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^{3}$ factorial design using a fixed fexofenadine concentration (50 ng/mL) with respect to its peak area and retention time. In addition, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 10-500 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of serum was 10 ng/mL, which was sensitive enough for the pharmacokinetic studies of terfenadine. The overall accuracy of the quality control samples ranged from 95.70 to 114.58% for fexofenadine with overall precision (% C.V.) being 3.53-14.39%. The relative mean recovery of fexofenadine for human serum was 90.17%. Stability studies (freeze-thaw, short-term, extracted serum sample and stock solution) showed that fexofenadine was stable during storage, or during the assay procedure in human serum. However, the storage at $-70^{\circ}C$ for 4 weeks showed that fexofenadine was not stable. The peak area and retention time of fexofenadine were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of fexofenadine in human serum samples for the pharmacokinetic studies of orally administered Tafedine tablet (60 mg as terfenadine) at three different laboratories, demonstrating the suitability of the method.

에토돌락 체내동태 연구를 위한 혈청 중 에토돌락의 HPLC 정량법 개발 및 검증 (Development and Validation of an HPLC Method for the Pharmacokinetic Study of Etodolac in Human)

  • 조혜영;강현아;문재동;최후균;이용복
    • Journal of Pharmaceutical Investigation
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    • 제35권4호
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    • pp.265-271
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    • 2005
  • A rapid, selective and sensitive reversed-phase HPLC method for the determination of etodolac in human serum was developed, validated, and applied to the pharmacokinetic study of etodolac. Etodolac and internal standard, ibuprofen were extracted from human serum by liquid-liquid extraction with hexane/isopropanol (95:5, v/v) and analyzed on a Luna C18(2) column with the mobile phase of 1% aqueous acetic acid-acetonitrile (4:6, v/v). Detection wavelength of 227 nm and flow rate of 1.0 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^3$ factorial design using a fixed etodolac concentration $(1\;{\mu}g/mL)$ with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of $0.05-40\;{\mu}g/mL$ with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of serum was 0.05 ${\mu}g/mL$, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the quality control samples ranged from 92.00 to 110.00% for etodolac with overall precision (% C.V.) being 1.08-10.11%. The percent recovery for human serum was in the range of 76.73-115.30%. Stability studies showed that etodolac was stable during storage, or during the assay procedure in human serum. The peak area and retention time of etodolac were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of etodolac in human serum samples for the pharmacokinetic studies of orally administered Lodin XL tablet (400 mg as etodolac) at three different laboratories, demonstrating the suitability of the method.

페노프로펜 체내동태 연구를 위한 혈청 중 페노프로펜의 HPLC 정량법 개발 및 검증 (Development and Validation of an HPLC Method for the Pharmacokinetic Study of Fenoprofen in Human)

  • 조혜영;강현아;김윤균;사홍기;이용복
    • Journal of Pharmaceutical Investigation
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    • 제35권6호
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    • pp.423-429
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    • 2005
  • A selective and sensitive reversed-phase HPLC method for the determination of fenoprofen in human serum was developed, validated, and applied to the pharmacokinetic study of fenoprofen calcium. Fenoprofen and internal standard, ketoprofen, were extracted from human serum by liquid-liquid extraction with diethyl ether and analyzed on a Luna C18(2) column with the mobile phase of acetonitrile-3 mM potassium dihydrogen phosphate (32:68, v/v, adjusted to pH 6.6 with phosphoric acid). Detection wavelength of 272 nm and flow rate of 0.25 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^{3}$ factorial design using a fixed fenoprofen concentration $(2\;{\mu}g/mL)$ with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of $0.05-100\;{\mu}g/mL$ with correlation coefficients greater than 0.999. The lower limit of quantification using 1 mL of serum was $0.05\;{\mu}g/mL$, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the quality control samples ranged from 92.27 to 109.20% for fenoprofen with overall precision (% C.V.) being 5.51-11.71 %. The relative mean recovery of fenoprofen for human serum was 81.7%. Stability (freeze-thaw, short and long-term) studies showed that fenoprofen was not stable during storage. But, extracted serum sample and stock solution were allowed to stand at ambient temperature for 12 hr prior to injection without affecting the quantification. The peak area and retention time of fenoprofen were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of fenoprofen in human serum samples for the pharmacokinetic studies of orally administered Fenopron tablet (600 mg as fenoprofen) at three different laboratories, demonstrating the suitability of the method.

디피리다몰 체내동태 연구를 위한 혈청 중 디피리다몰의 HPLC 정량법 개발 및 검증 (Development and Validation of an HPLC Method for the Pharmacokinetic Study of Dipyridamole in Human)

  • 조혜영;강현아;문재동;최후균;이용복
    • Journal of Pharmaceutical Investigation
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    • 제36권1호
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    • pp.45-51
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    • 2006
  • A rapid, selective and sensitive reversed-phase HPLC method for the determination of dipyridamole in human serum was developed, validated, and applied to the pharmacokinetic study of dipyridamole. Dipyridamole and internal standard, loxapine, were extracted from human serum by liquid-liquid extraction with diethyl ether and analyzed on a Nova Pak $C_{I8}$ column with the mobile phase of 40 mM ammonium acetate:methanol:acetonitrile (35:35:30)(v/v/v, pH 7.8). Detection wavelength of 280 nm and flow rate of 1.0 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^3$ factorial design using a fixed dipyridamole concentration (50 ng/mL) with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 2-2000 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of serum was 2 ng/mL, which was sensitive enough for pharmacokinetic studies of dipyridamole. The overall accuracy of the quality control samples ranged from 103.94 to 105.86% for dipyridamole with overall precision (% C.V.) being 4.60-11.49%. The relative mean recovery of dipyridamole for human serum was 97.64%. Stability studies showed that dipyridamole was stable during storage, or during the assay procedure in human serum. The peak area and retention time of dipyridamole were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of dipyridamole in human serum samples for the pharmacokinetic studies of orally administered Dimor tablet (75 mg as dipyridamole) at three different laboratories, demonstrating the suitability of the method.

염산프로메타진 체내동태 연구를 위한 혈청 중 프로메타진의 HPLC 정량법 개발 및 검증 (Development and Validation of HPLC Method for Pharmacokinetic Study of Promethazine in Human)

  • 조혜영;강현아;이화정;최후균;이용복
    • Journal of Pharmaceutical Investigation
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    • 제36권1호
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    • pp.23-29
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    • 2006
  • A rapid, selective and sensitive reversed-phase HPLC method for the determination of promethazine in human serum was developed, validated, and applied to the pharmacokinetic study of promethazine. Promethazine and internal standard, chlorpromazine, were extracted from human serum by liquid-liquid extraction with n-hexane containing 0.8% isopropanol and analyzed on a Capcell Pak CN column with the mobile phase of acetonitrile-0.2 M potassium dihydrogen phosphate (42:58, v/v, adjusted to pH 6.0 with 1 M NaOH). Detection wavelength of 251 nm and flow rate of 0.9 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^{3}$ factorial design using a fixed promethazine concentration (10 ng/mL) with respect to its peak area and retention time. In addition, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 1-40 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 1 mL of serum was 1 ng/mL, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the quality control samples ranged from 96.15 to 105.40% for promethazine with overall precision (% C.V.) being 6.70-11.22%. The relative mean recovery of promethazine for human serum was 63.54%. Stability (freeze-thaw and short-term) studies showed that promethazine was stable during storage, or during the assay procedure in human serum. However, the storage at $-80^{\circ}C$ for 4 weeks showed that promethazine was not stable. Extracted serum sample and stock solution were not allowed to stand at ambient temperature for 12 hr prior to injection. The peak area and retention time of promethazine were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of promethazine in human serum samples for the pharmacokinetic studies of orally administered Himazin tablet (25 mg as promethazine hydrochloride) at three different laboratories, demonstrating the suitability of the method.

환경 오염물질의 정량법 개발과 거동에 관한 연구 ( I ) : 미셀 역상 액체 크로마토그래피에서 페놀과 벤젠 일치환체들의 용리거동 (A Study on the Development of Analytical Methods and Behaviors of Environmental Pollutants ( I ) : Elution Behavior of Monosubstituted Phenols and Benzenes by Micellar Reversed-Phase Liquid Chromatography)

  • 이대운;방은정;조병연
    • 분석과학
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    • 제6권1호
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    • pp.1-8
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    • 1993
  • 음이온 계면활성제인 sodium dodecyl sulfate(SDS)를 이동상으로 한 미셀 액체 크로마토그래피(micellar liquid chromatography : MLC)에서, 시료로 22종의 페놀과 벤젠 일치환체들을 선택하여 이 시료들의 용리거동을 조사하여 MLC계에서의 소수성 효과를 알아 보았다. MLC에서의 머무름과 미셀 농도간의 상관관계를 통해 시료들이 미셀-물간, 변형된 정지상-물 사이에서 분배될 때의 분배계수를 구하였고, 또 이를 이용하여 물-미셀간의 전이 자유 에너지를 구하였다. 이러한 MLC에서 얻은 소수성 파라미터들은 옥탄올-물계와 연관시켜 본 결과 좋은 상관관계를 보였다. 따라서 이 두 계에서 시료의 소수성이 머무름에 중요한 영향을 미침을 알 수 있었다. 한편, MLC를 이용하면 quantitative structure activity relationships(QSAR)에서의 소수성 정량 연구에 적용이 가능하다. 또한 알킬 치환체들에서 탄소 수의 증가에 따른 머무름 관계를 통하여 소수성의 선택성을 알아 보았고, 유기 변형제로 n-프로판올을 첨가하였을 때에도 마찬가지로 MLC계에서의 소수성 파라미터와 옥탄올-물계 사이에 상관관계가 있음을 알았다.

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