• Title/Summary/Keyword: Relative precision

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Development of Quality Control Method for a Novel Herbal Medicine, HPL-1 using UHPLC (UHPLC를 이용한 새로운 한약제제 HPL-1의 품질관리법 개발)

  • Kim, Se-Gun;Lamichhane, Ramakanta;Lee, Kyung-Hee;Jung, Hyun-Ju
    • The Korea Journal of Herbology
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    • v.30 no.3
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    • pp.19-24
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    • 2015
  • Objectives : HPL-1, a novel herbal medicine which is composed of five herbs such as Kalopanacis Cortex, Chaenomelis Fructus, Raphani Semen, Atractylodis Rhizoma and Pulvis Aconiti Tuberis Purificatum, was developed for treatment of osteoarthritis. This study is aimed to develop analytical method for consistent quality control of HPL-1 and validate chromatographic method. Methods : Chromatographic analysis was performed using ultra-high performance liquid chromatography - diode array detector (UHPLC-DAD) equipped with RP-amide column, column oven, and auto sampler. Marker compounds [protocatechuic acid, chlorogenic acid, liriodendrin, 3,5-dicaffeoylquinic acid, ${\beta}$-D-(3-O-sinapoyl)-fructofuranosyl-$\alpha$-D-(6-O-sinapoyl)glucopyranoside and benzoylmesaconine] were separated by step gradient elution of acetonitrile and 0.1% phosphoric acid/water. The method validation was evaluated by quantitative validation parameters of linearity, accuracy, precision, limit of detection (LOD) and limit of quantification (LOQ) according to KFDA guideline.Results : An optimized method for six marker compounds in HPL-1 was established by UHPLC-DAD. The correlation coefficient (R2) with each calibration curve was greater than 0.99. The LOD and LOQ were within the range of 0.008-0.090 and $0.023-0.274{\mu}g/mL$, respectively. The relative standard deviation (RSD) of intra- and inter-day variability were less than 4.0%. The result of recovery test was range from 93.3-106.3% with RSD < 4.0%.Conclusions : These results suggest that the quantitative UHPLC method is precise, accurate, effective for quality evaluation of HPL-1. The method may also contribute to improve quality of crude drug preparations used for treatment of various diseases.

Atomization Characteristics in Pneumatic Counterflowing Internal Mixing Nozzle

  • Lee, Sam-Goo;Rho, Byung-Joon
    • Journal of Mechanical Science and Technology
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    • v.14 no.10
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    • pp.1131-1142
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    • 2000
  • In an effort to illustrate the global variation of SMD (Sauter mean diameter, or $D_{32}$) and AMD (Arithmetic mean diameter, or $D_{10}$) at five axial downstream locations (i. e., at Z=30, 50, 80, 120, and 170 mm) under the different experimental conditions, the radial coordinate is normalized by the spray half-width. Experimental data to analyze the atomization characteristics concerning with an internal mixing type have been obtained using a PDPA(Phase Doppler Particle Analyzer). The air injection pressure was varied from 40 kPa to 120 kPa. In this study, counterflowing internal mixing nozzles manufactured at an angle of $15^{\circ}$with axi-symmetric tangential-drilled four holes have been considered. By comparing the results, it is clearly possible to discern the effects of increasing air pressure, suggesting that the disintegration process is enhanced and finer spray droplets can be obtained under higher air assist. The variations in $D_{32}$ are attributed to the characteristic feature of internal mixing nozzle in which the droplets are preferentially ejected downward with strong axial momentum, and dispersed with the larger droplets which are detected in the spray centerline at the near stations and smaller ones are generated due to further subsequent breakup by higher shear stresses at farther axial locations. The poor atomization around the centre close to the nozzle exit is attributed to the fact that the relatively lower rates of spherical particles are detected and these drops are not subject to instantaneous breakup in spite of the strong axial momentum. However, substantial increases in SMD from the central part toward the edge of the spray as they go farther downstream are mainly due to the fact that the relative velocity of droplet is too low to cause any subsequent disintegration.

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The role of matrix modifier and for the determination of cadmium in blood by graphite furnace atomic absorption spectrometry (흑연로 원자흡수분광법에 의한 혈중 카드뮴 분석시 매트릭스 개선제(matrix modifier)의 역할)

  • Yoo, Kwang-Sik;Kim, Chang-Bok;Kwon, Jin-Kee
    • Analytical Science and Technology
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    • v.8 no.1
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    • pp.9-16
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    • 1995
  • The low concentration of cadmium in the whole-blood was determined by graphite furnace atomic absorption spectrometry(GFAAS) after the sample was diluted five-fold by 1% Triton X-100, 2% $(NH_4)_2HPO_4$ as matrix modifier and pyrocoated graphite tube with L'vov platform was tried remove the interferences of blood matrix and reduce the loss of volatility of cadmium at higher ashing temperature($600^{\circ}C$). The criteria for evaluating the accuracy and precision of this analysis was confirmed by analysis of interlaboratory comparison(Japan) and NIST SRM No. 909(Cd in Serum). The limit of the determination for cadium was 0.1ng/ml and the relative standard deviation(RSD) at 1.0ng/ml level was about 10% for the GFAAS.

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Determination of Absolute Coordinates of Permanent GPS Site (GPS 상시관측소의 절대좌표 산정에 관한 연구)

  • 윤홍식;황진상
    • Journal of the Korean Society of Surveying, Geodesy, Photogrammetry and Cartography
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    • v.19 no.4
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    • pp.415-423
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    • 2001
  • This paper deals with the data processing method relative to reference frames through the calculation of absolute coordinates of permanent GPS site which was established at Sungkyunkwan University. In this paper. we computed the ITRF97 coordinates with high precision (0.0001 ppm) from GPS data analysis. Also, we derived the accurate coordinates referred to WGS84 and Korean Geodetic Datum (KGD) using transformation parameters provided. ITRF97 coordinates were computed by using the GIPSY-OASIS II (GOA II) software and the algorithms for determining the position developed Jet Propulsion Laboratory (JPL). The coordinates referred to WGS84 and KGD were derived from the transformation parameters provided by International Earth Rotation Service (IERS) and National Geography Institute (NGI). The parameters determined by NGI were calculated from the 2000 project of the establishment of geocentric coordinate system. We tested its availability through the comparison of the coordinates obtained from local GPS data analysis.

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Simultaneous Determination of the Flavonoids and Limonoids in Citrus junos Seed Shells Using a UPLC-DAD-ESI/MS

  • Jo, Ara;Shin, Ji hun;Song, Hwa young;Lee, Ye Eun;Jeong, Da Eun;Oh, Sung Hwa;Mun, Myung Jae;Lee, Mina
    • Natural Product Sciences
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    • v.26 no.1
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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.

Development of high-performance liquid chromatography methods for the anticoccidials: toltrazuril and diclazuril (고속액체크로마토그래피를 이용한 항원충제 분석법 개발: 톨트라주릴 및 디클라주릴)

  • Jeong, Kyung Hun;Jeong, Miyoung;Park, Hae-Chul;Hossain, Md Akil;Kim, Daegyun;Lee, Kwang-Jick;Kang, Jeong Woo
    • Korean Journal of Veterinary Research
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    • v.57 no.4
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    • pp.223-226
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    • 2017
  • This study was undertaken to develop new analytical methods for assessment of anticoccidials. High-performance liquid chromatography (HPLC) was found to be a fast, reliable, and practical method. The anticoccidials used in this experiment were toltrazuril and diclazuril, and the analysis factors were specificity, linearity, accuracy, repeatability, and intermediate precision. The linearity of each anticoccidial was better than 0.99, and the accuracies were 99.5% and 99.1% with relative SD of 0.5 and 0.4, respectively. To assess whether the developed HPLC method could be effectively applied, toltrazuril and diclazuril post-market veterinary products (five products) that are currently sold were tested. The results revealed no non-compliant items and the method was applied successfully. Therefore, the newly developed HPLC method for anticoccidial assessment described in this study may be useful as a reference method in the Korean Standards of Veterinary Pharmaceuticals for the analysis of toltrazuril and diclazuril.

Palaeomagnetism of Early Cretaceous Sedimentary Rocks in Chingyo-Sach'ŏn Area, Southwestern Kyŏngsang Basin (경상분지 남서부 진교-사천 지역 전기백악기 퇴적암에 대한 고자기 연구)

  • Kim, In-Soo;Kang, Hee-Cheol;Lee, Hyun Koo
    • Economic and Environmental Geology
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    • v.26 no.4
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    • pp.519-539
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    • 1993
  • A total of 264 independently oriented core samples were collected from 26 sites in the southwestern part (the Naktong Trough) of the Cretaceous $Ky{\check{o}}ngsang$ Basin in south Korea. The sampled formations comprise the sedimentary Shindong and the Hayang Groups of the Lower Cretaceous age. Alternating field and thermal demagnetizations were conducted. Characteristic remanent magnetization (ChRM) was relatively easily isolated in each formation except in the Chinju formation, from which only remagnetization circles were observed. Even though an extensive use of the fold test was not possible due to the nearly homoclinal nature of the strata in the area, we believe that the ChRM of each formation is of primary origin based on the following grounds: The in-situ ChRM direction of each formation is different from the present geomagnetic field direction. Fisherian precision parameter becomes enhanced through the tilt correction in all formations, closely to the values required for a positive fold test. Three out of the five studied formations pass the reversal test. The mean palaeomagnetic pole position from the studied area is found to be statistically different from the contemporary pole from the Chinese block exclusive of the Shandong area. The difference in magnetic declination suggests a $14.5^{\circ}$ (${\pm}10.5^{\circ}$) clockwise rotation of the studied area relative to the Chinese block comprising the west of the Tan-Lu fault. On the other hand, any significant difference in magnetic inclination and concurrent palaeolatitude is not observed between the studied area and China as well as the other area (Taegu-Andong area) in the $Ky{\check{o}}ngsang$ Basin. The dual nature of the magnetic polarity confirmed in all formations suggests an older than 124 Ma (Neocomian or older) age of the studied sedimentary strata.

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HPLC Validation of Valerian Ethanol Extract as a Functional Food (건강기능식품 원료로서 길초근 주정 추출물의 지표성분 분석법 검증)

  • Jo, Kyungae;Han, Sung Hee;Bae, Song-Hwan;Shin, Jung Cheul;Suh, Hyung Joo
    • The Korean Journal of Food And Nutrition
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    • v.31 no.1
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    • pp.104-108
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    • 2018
  • The purpose of this study was to establish valerenic acid as a marker compound for the standardization of ethanol extract of Valerinan officinalis (valerian) root as a functional health food. We established valerenic acid as a marker compound using HPLC. HPLC was used to quantify the marker compound in the valerian extract after validation of methods with linearity, accuracy, and precision. The specificity for retention time was met by comparative analysis of the valerian extract and standard compound using HPLC. The method showed high linearity of the calibration curve with a coefficient of correlation ($R^2$) of 0.9999. The limit of quantification (LOQ) was $10{\mu}g/mL$. The accuracy of measurement was 99.88~00.68% and the relative standard deviation (RSD) value was 0.59%. In addition, our analytical method yielded a 29% mean content of valerenic acid in the valerian ethanol extract. These results indicate that the established HPLC method facilitated the determination of marker compounds in the valerian extract for the standardization of health functional foods.

Determination of Selenium in Milk by ICP-OES (ICP-OES를 이용한 우유의 Selenium 분석)

  • 김효중;박종길;신정걸;백영진
    • Food Science of Animal Resources
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    • v.23 no.4
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    • pp.356-360
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    • 2003
  • The purpose of this paper was to determine the quantity of selenium in milk by inductively coupled plasma optical emission spectrometry. The sample was digested in teflon vessel containing nitric-hydrogen peroxide acid mixture. After digestion, the sample is treated with additional hydrochloric acid. Total selenium was reduced with sodium borohydride and concentrated hydrochloric acid in a simplified hydride generation(HG) manifold. The optimum conditions of HG are 2 M for HCl, 1.5% for NaBH$_4$, 1.2 mL/mim for sample flow. Recovery rates by the standard addition method were 88.0% at 10 ppb and 92.2% at 10 ppm. The relative standard deviations were 4.8 and 3.2%, respectively. This method showed a good accuracy and precision. And so it was highly suitable for determination of small quantity of selenium in milk.

Implementation of Z-Factor Statistics for Performance Evaluation of Quality Innovation in the High Throughput Process (High Throughput 프로세스에서 품질혁신의 성능평가를 위한 Z-Factor의 적용방안)

  • Choi, Sung-Woon
    • Journal of the Korea Safety Management & Science
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    • v.15 no.1
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    • pp.293-301
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    • 2013
  • The purpose of this study is to introduce the limit of previously used six sigma quality process evaluation metrics, $Z_{st}$ and $P_{pk}$, and a solution to overcome this drawback by using a metric based on performance evaluation of Z-factor quality innovation. Case analysis on projects from national six sigma contest from 2011 to 2012 is performed and literature review on new drug development HTS (High Throughput Screening) is used to propose innovative performance evaluation metrics. This research shows that experimental study on six sigma evaluation metric, $Z_{st}$ and $P_{pk}$, have no significance difference between industrial type (Manufacturing, Semi-Public Institute, Public Institute) and CTQ type (Product Technology Type CTQ, Process Technology Type CTQ). Following discovery characterize this quality improvement as fixed target type project. As newly developed moving target type of quality innovation performance metric Z-Factor is used for evaluating experimental study, hypothetical analysis suggests that $Z_{st}$ and $P_{pk}$ share different relationship or even show reciprocal relationship. Constraints of the study are relatively small sample size of only 37 projects from past 2 years and conflict on having interview and communication with six sigma quality practitioner for qualitative experimental study. Both moving target type six sigma innovation project and fixed target type improvement project or quality circle enables efficient ways for a better understanding and quality practitioner use by applying quality innovation performance metric. Downside of fixed target type quality performance evaluation metric, $Z_{st}$ and $P_{pk}$, is presented through experimental study. In contrast, advantage of this study is that high throughput requiring product technology, process technology and quantum leap typed innovation effect is evaluated based on precision and accuracy and Z-Factor that enables relative comparison between enterprises is proposed and implemented.