• 생약학회지
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• 제45권4호
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• pp.294-299
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• 2014

The simultaneous determination of platyphylloside, aceroside and betulin was established for the quality control of Betula platyphylla bark using a high performance liquid chromatography and diode-array UV/Vis detector (HPLC-DAD). Separation and quantification were successfully achieved with a INNO C18 column ($5{\mu}m$, 4.6 mm $I.D.{\times}150mm$) by gradient elution of a mixture of methanol and water at a flow rate of 1.0 ml/min. Validation of the developed method was performed by various factor such as linearity, specificity, precision, accuracy, system suitability and stability. This method was successfully applied to the determination of contents of platyphylloside, aceroside VIII and betulin in three batches of Betula platyphylla bark extract. These results suggest that the developed HPLC method is simple, effective and could be utilized as a quality control method for Betula platyphylla bark products.

• Journal of the Optical Society of Korea
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• 제18권4호
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• pp.301-306
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• 2014

A porous silicon microcavity (PSMC) sensor has been made for vapors of solvent solutions, and a method has been developed in order to obtain simultaneous determination of two volatile substances with different concentrations. In our work, the temperature of the solution and the velocity of the air stream flowing through the solution have been used to control the response of the sensor for ethanol and acetone solutions. We study the dependence of the cavity-resonant wavelength shift on solvent concentration, velocity of the airflow and solution temperature. The wavelength shift depends linearly on concentration and increases with solution temperature and velocity of the airflow. The dependence of the wavelength shift on the solution temperature in the measurement contains properties of the temperature dependence of the solvent vapor pressure, which characterizes each solvent. As a result, the dependence of the wavelength shift on the solution temperature discriminates between solutions of ethanol and acetone with different concentrations. This suggests a possibility for the simultaneous determination of the volatile substances and their concentrations.

• 약학회지
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• 제51권3호
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• pp.174-178
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• 2007

A reverse-phase high performance liquid chromatography method with electrospray ionization and detection by mass spectrometry is described for the simultaneous determination of doxifluridine and its active metabolite 5-flu-orouracil (5-FU) in monkey serum. The method has greater sensitivity and simpler process than previous published methods with good accuracy and precision. A proper liquid/liquid extraction was used to extract simultaneously doxifluridine and 5-FU which has considerable difference in the polarity. Extracts were analyzed using LC/MS/MS providing a short analysis time within 5 min. The lower limit of quantification was validated at 10.0 ng/ml of serum for both doxifluridine and 5-FU. Accuracy and precision of quality control (QC) samples for both analytes met FDA Guidance criteria of ±15% for average QC accuracy with coefficients of variation less than 15%. The method will be applicable for preclinical studies and bioequivalence studies.

• 대한화학회지
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• 제33권2호
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• pp.208-214
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• 1989

구리(Ⅱ)와 코발트(Ⅱ)의 테트라 티오시안 착이온은 Amberlite LA 1, Alamine 336 또는 Aliquat 336과 같은 고분자량 알킬아민과 이온쌍 화합물이 형성되면 붉은색과 푸른색을 띠어 파장 480nm와 625nm에서 각각 최대 흡수 봉우리를 나타내므로 같은 조건에서 이들 이온쌍 화합물을 methyl isobutyl ketone으로 동시 추출하여 분광광도법으로 두 금속원소를 동시 정량하는 방법을 기술하였다. 그러나 각 흡수스펙트럼이 서로 조금씩 겹치기 때문에 흡광도로부터 농도를 구하기 위하여는 두개의 연립방정식이 필요했다. Fe(Ⅲ)와 Ni(Ⅱ)은 적은 양이 공존하더라도 구리 정량에 영향을 주었다. 이 동시정량법에 의해서 강철과 광물시료의 분석결과는 구리와 코발트 원소를 각각 분석한 결과와 잘 일치하였다.

• 대한본초학회지
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• 제25권3호
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• pp.65-71
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• 2010

Objectives：To develop and validate HPLC-PDA methods for simultaneous determination of seven constituents in Samchulkunbi-tang (SKT). Additionally, we investigated the cytotoxicity against BEAS-2B cell line and splenocytes of SKT. Methods：Reverse-phase chromatography using a Gemini $C_{18}$ column operating at $40^{\circ}C$, and photodiode array (PDA) detection at 230, 254 and 280 nm, were used for quantification of the three marker components of SKT. The mobile phase using a gradient flow consisted of two solvent systems. Solvent A was 1.0% (v/v) aqueous acetic acid and solvent B was acetonitrile with 1.0% (v/v) acetic acid. The cytotoxicity of SKT were measured by the CCK-8 assay method. Results：Calibration curves were acquired with $r^2$>0.9999, and the relative standard deviation (RSD) values (%) for intra- and inter-day precision were less than 6.0%. The recovery rate of each compound was in the range of 86.89-109.78%, with an RSD less than 4.0%. The contents of seven compounds in SKT were 1.39-6.84 mg/g. SKT had no cytotoxicity effect at 50-200 ${\mu}g$/mL concentrations. Conclusions：The established method will be helpful to improve quality control and in vitro efficacy study of SKT.

• Natural Product Sciences
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• 제22권4호
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• pp.238-245
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• 2016

Gumiganghwal-tang has been used for the treatment of common cold for a long-time. We developed an accurate and sensitive high performance liquid chromatography-diode array detection (HPLC-DAD) and electrospray ionization mass spectrometry method for the simultaneous determination of ferulic acid, baicalin, bergapten, methyl eugenol, glycyrrhizin, oxypeucedanin, wogonin, nodakenin, atractylenolide III, imperatorin, and atractylenolide I in Gumiganghwal-tang samples. The analytes were separated on a Shiseido C18 column ($5{\mu}m$, $4.6mm\;I.D.{\times}250mm$) with gradient elution with acetonitrile and 0.1% trifluoroacetic acid. Eleven compounds were quantitatively determined by HPLC-DAD and identified by LC-MS data. We also validated this method. The calibration curves of all the compounds showed good linear regression. The limits of detection and the limits of quantification ranged from 0.04 to 0.63 and from 0.12 to $1.92{\mu}g/mL$, respectively. The relative standard deviation values of intra- and inter-days of this method represented less than 2.9%. The recoveries were found to be in the range of 90.06 - 107.66%. The developed method has been successfully applied to the analysis of Gumiganghwaltang samples. The established HPLC method could be used to quality control of Gumiganghwal-tang.

• 분석과학
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• 제31권2호
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• pp.88-95
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• 2018

A simple, sensitive, and selective high-performance liquid chromatography (HPLC) method was developed and validated for the simultaneous quantification of fluorometholone (FLU) and tetrahydrozoline hydrochloride (THZ) in combined ophthalmic formulations. The effects of several factors, including detection wavelength, buffer pH, buffer concentration, and organic solvent concentration, on the performance of the method were investigated. The performance of the developed method was validated in accordance with the requirements of the International Conference on Harmonization. The linearity of the calibration curves in the desired concentration range was high for both FLU and THZ ($r^2=0.9999$). The accuracy and precision of the method were determined by a recovery study at analyte concentrations of 80 %, 100 %, and 120 %. The recovery was 99.60-100.17 % for both analytes, with a relative standard deviation less than 1.0 % at any concentration level. The validated results indicate that the new HPLC method could be successfully applied for the simultaneous determination of FLU and THZ in ophthalmic suspensions.

• Natural Product Sciences
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• 제26권1호
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• pp.64-70
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• 2020

Citrus junos seeds (CS) have been traditionally used for the treatment of cancer and neuralgia. They are also used to manufacture edible oil and cosmetic perfume. A large amount of CS shells without oil (CSS) are discarded after the oil in CS is used as foods or herbal remedy. To efficiently utilize CSS as a by-products, it needs to be studied through chemical analysis. Therefore, we developed an ultra-performance liquid chromatography (UPLC)-diode array detection (DAD) method for simultaneous determination and quantitative analysis of five components (two flavonoids and threes limonoids) in CSS. A Waters Acquity UPLC HSS T3 column C18 (2.1 × 100 mm, 1.8 ㎛) was used for this separation. It was maintained at 40 ℃. The mobile phase used for the analysis was distilled water and acetonitrile with gradient elution. To identify the quantity of the five components, a mass spectrometer (MS) with an electrospray ionization (ESI) source was used. The regression equation showed great linearity, with correlation coefficient ≥ 0.9912. Limits of detection (LOD) and limits of quantification (LOQ) of the five compounds were 0.09 - 0.13 and 0.26 - 0.38 ㎍/mL, respectively. Recoveries of extraction ranged from 97.45% to 101.91%. Relative standard deviation (RSD) values of intra- and inter-day precision were 0.06 - 1.15% and 0.19 - 0.25%, respectively. This UPLC-DAD method can be validated to simultaneously analyze quantities of marker flavonoids and limonoids in CSS.

• 한국식품과학회지
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• 제37권6호
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• pp.1024-1027
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• 2005

본 연구에서는 성장기용 조제식 중에 영양강화를 위해 첨가하는 비타민 $D_3$와 $K_1$의 함량측정을 위해 lipase를 이용하여 효소 가수분해 후 유기용매로 비타민을 추출하여 동시에 분석하는 신속분석법을 위와 같이 수행하였다. 추출된 비타민을 전처리 컬럼에서 2번의 switching time을 설정하여 농축컬럼에 홉착시킨 후 gradient mode로 2가지 이동상으로 분석컬럼에서 각각의 성분을 모두 분리하여 동시에 검출하는 방법을 사용하였다. 시료로 사용된 성장기용 조제식은 표기함량보다 다소 높게 분석되었으나, 국제표준인증물질을 시료로 사용하여 본 연구의 실험방법에 의해 측정된 값은 인증된 표준값내의 결과를 보여주었다. 따라서, 비타민 $D_3$ 또는 $K_1$을 강화한 분유, 이유식 등의 분말 유제품 중에서 함량을 측정하고자 할 때 한정된 장비와 인력으로 각각의 2가지 실험방법을 수행하기가 어렵거나 시간단축이 필요한 경우, 본 연구에서 수행한 실험방법과 같이 시료전처리를 간단하고 신속하게 수행할 뿐만 아니라 역상컬럼과 column-switching HPLC에 의해 비타민 $D_3$ 또는 $K_1$을 동시에 분석함으로써 보다 효율적인 분석을 진행 할 수 있을 것으로 사료된다.

• 약학회지
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• 제52권2호
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• pp.93-100
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• 2008

A liquid chromatographic method with tandom spectrometric detection (LC/MS/MS) for the simultaneous determination of doxifluridine and its active metabolite, 5-fluorouracil (5-FU) was developed over the concentration range of $5{\sim}2000$ ng/ml, respectively. Doxifluridine, 5-FU and internal standard, 5-chlorouracil (5-CU), were extracted from liver and intestine tissue via protein precipitation. Acetonitrile was used as the extraction solvent and the supernatant was evaporated and reconstructed in mobile phase. Optimum chromatographic separation was achieved on a Agilent Zorbax $C_{18}$ ($100\;mm{\times}2.1\;mm$, $3.5\;{\mu}m$) column with mobile phase run in isocratic with methanol : water (20 : 80, v/v). The flow rate was 0.2 ml/min with total cycle time of 5 min. The lower limit of quantification was validated at 5.0 ng/ml of liver and intestine tissue, for both doxifluridine and 5-FU, respectively. The intra-day and inter-day precision and accuracy of quality control (QC) samples were <11% coefficient of variation and <7% relative error from theoretical concentration for both analytes. In addition, the special designed stability study was performed, because the metabolism of doxifluridine occurs spontaneously even in ice bath for monkey liver. The stability of doxifluridine in liver and intestine of monkey and beagle dog was compared. It was found that bioanalytical validation could not be performed for the monkey liver; however, beagle dog's liver has relatively low speed of metabolism compared to monkey liver and instead of monkey liver, beagle dog's liver could be used for the validation. Bioanalytical validation could be performed in monkey intestine. Eventually, this developed method for liver and intestine will be useful in support of the toxicokinetic and pharmacokinetic studies of doxifluridine and 5-FU.