• Title/Summary/Keyword: Analytical Validation

Search Result 584, Processing Time 0.037 seconds

Method Validation for the Simultaneous Analysis of Organophosphorous Pesticides in Blood by GC/MS (GC/MS를 이용한 혈액 중 유기인제류 농약의 동시 분석에 관한 방법의 유효화)

  • Park Mee Jung;Yang Ja Youl;Kim Ki Wook;Park Yoo Shin;Chung Hee Sun;Lee Sang Ki
    • Environmental Analysis Health and Toxicology
    • /
    • v.20 no.4 s.51
    • /
    • pp.297-302
    • /
    • 2005
  • The purpose of this study was to provide the standard method for the analysis of organophosphorous pesticides such as chlorpyrifos, diazinon, malathion and parathion in blood. We performed method validation for these pesticides in blood according to EURACHEM (A focus For Analytical Chemistry in Europe) guide. For the analysis of the pesticides, we used solid-phase extraction ,column (Waters Oasis $HLB^{(R)}$. After the extraction, the supernatants were evaporated to dryness under the nitrogen stream. They were analyzed by gas chromatography/mass spectrometry (GC/MS) after reconstituting with ethanol. Terbufos was used as an internal standard. To validate this method, we performed verification procedures with the following parameters: selectivity, linearity of calibration, accuracy, precision, limit of detection and quantification. Validation data according to Eurachem guide were adequate for our purpose for the analysis of chlorpyrifos, diazinon, malathion and parathion in blood.

Development of HPLC assay method of fusidate sodium tablets

  • Lee, GaJin;Choi, Min;Truong, Quoc-Ky;Mai, Xuan-Lan;Kang, Jong-Seong;Woo, Mi Hee;Na, Dong-Hee;Chun, In-Koo;Kim, Kyeong Ho
    • Analytical Science and Technology
    • /
    • v.30 no.3
    • /
    • pp.154-158
    • /
    • 2017
  • The Korean Pharmacopoeia (KP XI), British Pharmacopoeia (BP 2013) and Japanese Pharmacopoeia contain monographs for the quality control of raw fusidate sodium and its formulations using high performance liquid chromatography (HPLC). However, the assay method for the determination of fusidate sodium in commercial tablets is titration which is less specific than HPLC. In this study, we present an alternative HPLC method for quantitation of fusidate sodium in tablets. Method validation was performed to determine linearity, precision, accuracy, system suitability, and robustness. The linearity of calibration curves in the desired concentration range was high ($r^2=0.9999$), while the RSDs for intra- and inter-day precision were 0.25-0.37 % and 0.11-0.60 %, respectively. Accuracies ranged from 99.46-100.85 %. Since the system suitability, intermediate-precision and robustness of the assay were satisfactory, this method will be a valuable addition to the Korean Pharmacopoeia (KP XI).

Development of Analytical Method of Biotin in Complex Drugs and Dietary Supplements Using HPLC-UV

  • Huh, Yoon-Young;Kang, Yun-Pyo;Choi, Yong-Seok;Park, Jeong-Hill;Kwon, Sung-Won
    • Journal of Pharmaceutical Investigation
    • /
    • v.41 no.1
    • /
    • pp.25-30
    • /
    • 2011
  • Recently, Korean Food and Drug Administration (KFDA) has focused on developing quality control guidelines for all commercial products in Korea to enforce regulations, improve the quality control, and protect consumers by developing prevalently used and efficient analytical tools to determine and quantify target compounds. Because the Korean Pharmacopeia (KP) presents microbiological assays for biotin, which is laborious and time-consuming, this study is focused on applying HPLC-UV to detect and quantify biotin in complex drugs and dietary supplements like multi-vitamin. Biotin in complex drugs was extracted from methanol and analyzed using mobile phase with 10 mM potassium phosphate (monobasic, pH=3.0) in distilled water and acetonitrile. Gradient condition was used to successfully detect and quantify biotin within 20 minutes. Validation result for linearity was significant that average $r^2$ was 0.999 (n=3) and its relative standard deviation (RSD) was 0.0578% which was less than 2%. Using this method, quantification of biotin in complex drugs was completed successfully and recovery tests were finished that recovery percentage greater than 95% with relative standard deviation less than 2%.

Development and Validation of Crocidolite Quality Control Samples for Proficiency Analytical Testing (청석면 분석 정도관리용 표준시료 개발 및 평가)

  • Lee, Ji-Hyun;Kim, Eun-Young;Noh, Su-Jin;Park, Yong-Jin;Jeong, Jee-Yeon
    • Journal of Environmental Health Sciences
    • /
    • v.37 no.1
    • /
    • pp.57-63
    • /
    • 2011
  • Crocidolite quality control (QC) sampling created by the wet generation method has been validated by validation tests such as the accuracy, precision, and storage tests. For this study we designed and developed a manufacturing apparatus and standard operating procedure for making these QC samples. The most important step in the procedure of making QC samples was the stage eliminating static electricity in asbestos fibers. This static electricity hampers the fibers clog functioning. In accuracy and precision tests by phase contrast microscopy analysis, the difference between the reference values and the studied values was at maximum 17.8%. This satisfies the AIHA proficiency analytical test criteria for asbestos. We could confirm the nearly even distribution of crocidolite fibers on the membrane filter. Also, there was no loss of fibers in the storage test after the one month.

Method development and validation for dieckol in the standardization of phlorotannin preparations

  • Kim, Jiyoung;Um, Minyoung;Yang, Hyejin;Kim, Inho;Lee, Changho;Kim, Yuntai;Yoon, Minseok;Kim, Youngkyoung;Kim, Jimi;Cho, Suengmok
    • Fisheries and Aquatic Sciences
    • /
    • v.19 no.1
    • /
    • pp.3.1-3.6
    • /
    • 2016
  • Phlorotannins are reported to have diverse biological properties. However, no analytical methods for the standardization of phlorotannin preparations have been reported. Herein, we developed and validated an analytical method for the determination of dieckol in phlorotannin extracts (PRT) using high-performance liquid chromatography (HPLC). The optimum HPLC conditions consisted of a Supelco Discovery C18 column stationary phase, a mobile phase (A: 15 % HPLC grade methanol in deionized water, B: methanol), UV detection at 230 nm, and a flow rate of 0.7 mL/min. The optimized chromatographic conditions were validated and exhibited good specificity and linearity ($R^2$ > 0.9994-1.0000). The recoveries were in the range of 100.9-102.3 %. The method had good intermediate (%RSD 1.2) and intra-day (%RSD 0.4-1.7) assay precisions. This HPLC method had good accuracy and quality in the determination of dieckol in PRT.

An HPLC method for the determination of thioctic acid in raw material and tablets

  • Mai, Xuan-Lan;Ahn, GyeChan;Lee, SeokHan;Kang, Jong-Seong;Woo, Mi Hee;Na, Dong-Hee;Chun, In-Koo;Kim, Kyeong Ho
    • Analytical Science and Technology
    • /
    • v.30 no.5
    • /
    • pp.221-225
    • /
    • 2017
  • Thioctic acid is a vitamin-like antioxidant which is prepared as tablets and injection. The Korean Pharmacopoeia (KP XI) contains monograph for the quality control of raw thioctic acid using ultra-violet visible spectrophotometry and its formulations using high performance liquid chromatography (HPLC). In British Pharmacopoeia 2013 (BP2013), another HPLC method is used for the assay test of thioctic acid material. For the international harmonization, we present an HPLC method for quantitation of thioctic acid in both raw material and tablets. Method validation was performed to determine linearity, precision, accuracy, system suitability, and robustness. The linearity of calibration curves in the desired concentration range was high ($r^2=0.9995$), while the RSDs for intra- and inter-day precision were 0.93 ~ 1.26 % and 1.40 ~ 1.76 %, respectively. Accuracies ranged from 98.13-100.00 %. Since the system suitability, intermediate-precision and robustness of the assay were satisfactory, this method will be a valuable addition to the Korean Pharmacopoeia (KP XI).

Solution verification procedures for modeling and simulation of fully coupled porous media: static and dynamic behavior

  • Tasiopoulou, Panagiota;Taiebat, Mahdi;Tafazzoli, Nima;Jeremic, Boris
    • Coupled systems mechanics
    • /
    • v.4 no.1
    • /
    • pp.67-98
    • /
    • 2015
  • Numerical prediction of dynamic behavior of fully coupled saturated porous media is of great importance in many engineering problems. Specifically, static and dynamic response of soils - porous media with pores filled with fluid, such as air, water, etc. - can only be modeled properly using fully coupled approaches. Modeling and simulation of static and dynamic behavior of soils require significant Verification and Validation (V&V) procedures in order to build credibility and increase confidence in numerical results. By definition, Verification is essentially a mathematics issue and it provides evidence that the model is solved correctly, while Validation, being a physics issue, provides evidence that the right model is solved. This paper focuses on Verification procedure for fully coupled modeling and simulation of porous media. Therefore, a complete Solution Verification suite has been developed consisting of analytical solutions for both static and dynamic problems of porous media, in time domain. Verification for fully coupled modeling and simulation of porous media has been performed through comparison of the numerical solutions with the analytical ones. Modeling and simulation is based on the so called, u-p-U formulation. Of particular interest are numerical dispersion effects which determine the level of numerical accuracy. These effects are investigated in detail, in an effort to suggest a compromise between numerical error and computational cost.

Analytical Method Validation of (-)Epicatechin gallate in Penthorum chinense Pursh Extract using HPLC

  • Kwon, Jin Gwan;Jung, Yeon Woo;Seo, Changon;Hong, Seong Su;Lee, Ji Eun;Shin, Hyun Tak;Jung, Su Young;Choi, Chun Whan;Kim, Jin Kyu
    • Proceedings of the Plant Resources Society of Korea Conference
    • /
    • 2019.04a
    • /
    • pp.100-100
    • /
    • 2019
  • This study attempted to establish a High Performance Liquid Chromatography (HPLC) analysis method for the determination of (-)-epicatechin gallate as a part of the quality control for the development of functional cosmetic materials from Penthorum chinense Pursh extracts. HPLC was performed on a Unison US-C18 column ($4.6{\times}250mm$, $5{\mu}m$) with a gradient elution of 0.05% (v/v) trifluoroacetic acid (TFA) and methyl alcohol at a flow rate of 1.0 mL/min at $30^{\circ}C$. The analyte was detected at 280 nm. The HPLC method was performed in accordance with the International Conference on Harmonization (ICH) guideline (version 4, 2005) of analytical procedures with respect to specificity, precision, accuracy, and linearity. The limits of detection and quantitation were 0.11 and 0.33 mg/mL, respectively. Calibration curves showed good linearity (r2 > 0.9999), and the precision of analysis was satisfied (less than 0.6%). Recoveries of quantified compounds ranged from 99.51 to 101.92%. This result indicates that the established HPLC method is very useful for the determination of marker compound in P. chinense Pursh extracts.

  • PDF

Optimization and validation of HPLC/DAD method for the determination of adenosine and cordycepin in cordyceps products

  • Sasikarn Panpraneecharoen;Tisorn Chatrakoon;Sompong Sansenya;Saowapa Chumanee
    • Analytical Science and Technology
    • /
    • v.36 no.4
    • /
    • pp.152-160
    • /
    • 2023
  • Adenosine and cordycepin are bioactive compounds with health benefits. Therefore, both substances are often used to assess the quality of Cordyceps products. Optimization and validation of the HPLC/DAD method for determining two nucleosides were studied. The samples were prepared using an ultrasound-assisted extraction (ultrasonic bath). The result was optimal conditions for aqueous extraction, an extraction time of 35 min, and an extraction temperature of 40 ℃. The Chromatographic separation was achieved using a reverse phase column (InfinityLab Poroshell 120 EC-C18, 4.6 × 250 mm, 2.7 ㎛) at 30 ℃ with a mobile phase gradient elution of water and methanol at a flow rate of 0.7 mL/min. The eluents were monitored via a diode array detector at 260 nm. Two nucleosides were separated by less than 12 min after injection. The developed method was found to be excellent linear (r2 > 0.9999), accurate (% recovery 95.34-98.51), and precise (% relative standard deviation < 2.0). The limit of detection (LOD) and quantification (LOQ) were 0.45 and 1.38 mg/mL for adenosine and 0.47 and 1.43 mg/mL for cordycepin, respectively. This method was satisfactory for simultaneously quantitating two nucleoside contents, which were used to evaluate Cordyceps products.

Study of an analytical model for screw loosening mechanism of dental implants (치과용 임플란트의 풀림현상 규명을 위한 해석적 모델에 관한연구)

  • Seo, June-Woo;Kang, Kyoung-Tak;Chun, Heoung-Jae;Han, Chong-Hyeon
    • Proceedings of the KSME Conference
    • /
    • 2007.05a
    • /
    • pp.636-641
    • /
    • 2007
  • This research focuses on the development of an analytical model loosening mechanism of dental implant system. The model is utilized for predictions of preload values for internal and external types of implants. It identifies the effects of various parameters such as friction, geometric factors and mechanical properties on the loosening mechanism of the implant system. The results of analytical model are compared to those of the numerical method for validation.

  • PDF