• Title/Summary/Keyword: linearity test

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Determination of PFOS in LDPE and the Result for Proficiency Testing (LDPE 중 PFOS의 분석법 개발과 비교숙련도 결과)

  • Jung, Jae Hak;Lee, Young Kyu;Myung, Seung Woon;Cheong, Nam Yong
    • Journal of the Korean Chemical Society
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    • v.57 no.1
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    • pp.40-51
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    • 2013
  • In order to develop a quantitation method for Perfluorooctanesulfonic acid(PFOS) contained in plastics that are mainly used in electric and electronic equipment, this study consisted of conducting method validations with LDPE samples using soxhlet solvent extraction and LC/MS. As a result, the limits of detection and quantitation (LOD, LOQ) were $2.58{\mu}g/L$ and $7.82{\mu}g/L$, respectively. Additionally, the recovery was 96-102%. For the correlation coefficient of LC/MS, the $r^2$ value was 0.9992 in the concentration range of $7.82-100{\mu}g/L$, which confirmed its linearity. Furthermore, for the standardization of the analysis method for PFOS in electric and electronic equipment to correspond to EU environmental regulations, we conducted a proficiency test with a number of domestic and international testing laboratories. Three of the ten testing laboratories that participated in the proficiency test submitted outliers. Accordingly, we examined the cause of the outliers using the $^{19}F$ NMR, finding that the main cause was an error in the processing of the results for isomers in PFOS that existed in standard solutions and samples.

Bioequivalence of Atorva Tablet® to Lipitor Tablet® (Atorvastatin 20 mg) (리피토정® (아토르바스타틴 20 mg)에 대한 아토르바정®의 생물학적동등성)

  • Lim, Hyun-Kyun;Lee, Tae-Ho;Lee, Jae-Hyun;Youm, Jeong-Rok;Song, Jin-Ho;Han, Sang-Beom
    • Journal of Pharmaceutical Investigation
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    • v.38 no.2
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    • pp.135-142
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    • 2008
  • The present study describes the evaluation of the bioequivalence of two atorvastatin tablets, Lipitor $Tablet^{(R)}$ (Pfizer, reference drug) and Atorva $Tablet^{(R)}$ (Yuhan, test drug), according to the guidelines of Korea Food and Drug Administration (KFDA). Forty-nine healthy male Korean volunteers received each medicine at the atorvastatin dose of 40 mg in a $2{\times}2$ crossover study with a two weeks washout interval. After drug administration, serial blood samples were collected at a specific time interval from 0-48 hours. The plasma atorvastatin concentrations were monitored by an high performance liquid chromatography -tandem mass spectrometer (LC-MS/MS) employing electrospray ionization technique and operating in multiple reaction monitoring (MRM) and positive ion mode. The total chromatographic run time was 4.5 min and calibration curves were linear over the concentration range of 0.1-100 ng/mL for atorvastatin. The method was validated for selectivity, sensitivity, linearity, accuracy and precision. $AUC_t$ (the area under the plasma concentration-time curve from time zero to 48hr) was calculated by the linear log trapezoidal rule method. $C_{max}$ (maximum plasma drug concentration) and $T_{max}$ (time to reach $C_{max}$) were complied trom 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 Atorva $Tablet^{(R)}$ / Lipitor $Tablet^{(R)}$ were ${\log}\;0.9413{\sim}{\log}\;1.0179$ and ${\log}\;0.831{\sim}{\log}\;1.0569$, respectively. These values were within the acceptable bioequivalence intervals of ${\log}\;0.8{\sim}{\log}\;1.25$. Based on these statistical considerations, it was concluded that the test drug, Atorva $Tablet^{(R)}$ was bioequivalent to the reference drug, Lipitor $Tablet^{(R)}$.

The Study on Applicability of Semi-conductive Compound for Radioactive Source Tracing Dosimeter in NDT Field (비파괴 검사 분야의 방사성 동위원소 위치추적을 위한 반도체 화합물의 적용 가능성 연구)

  • Shin, Yohan;Han, Moojae;Jung, Jaehoon;Kim, Kyotae;Heo, Yeji;Lee, Deukhee;Cho, Heunglae;Park, Sungkwang
    • Journal of the Korean Society of Radiology
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    • v.13 no.1
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    • pp.39-44
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    • 2019
  • Radiation safety management is being considered very important since radioactive isotopes such as Co-60 and Ir-192 are widely used in fields such as non-destructive test(NDT). In this study, the applicability of Mercury(II) Iodide($HgI_2$) source for tracing system was evaluated. To make sure the unit cell sensor's reliability, we evaluated the electrical properties of the sensor made with $HgI_2$, and then position dependence of the sensor was analyzed and compared with the dose distribution from the planning system. As a result of the evaluation, high reliability of the sensor was shown through the linearity of R-sq > 0.990 and reproducibility of CV < 0.015. In the position dependence evaluation, the maximum value was measured at the isocenter of the sensor and gradually decreased according to the distance. However, the dose distribution data from the planning system was turned out that has difference with that of the sensor up to 30%. This seems to come from the difference between single-point measuring based planning system and area measuring based sensor.

Exposure Assessment of Heavy Metals Migrated from Glassware on the Korean Market (국내 유통 식품용 유리제의 중금속 노출 평가)

  • Kim, Eunbee;Hwang, Joung Boon;Lee, Jung Eun;Choi, Jae Chun;Park, Se-Jong;Lee, Jong Kwon
    • KOREAN JOURNAL OF PACKAGING SCIENCE & TECHNOLOGY
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    • v.28 no.1
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    • pp.15-21
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    • 2022
  • The purpose of our study was to investigate the migration level of lead (Pb), cadmium (Cd), and barium (Ba) from glassware into a food simulant and to evaluate the exposure of each element. The test articles were glassware, including tableware, pots, and other containers. Pb, Cd, and Ba were analysed by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). The analytical performance of the method was validated in terms of its linearity, limit of detection (LOD), limit of quantification (LOQ), recovery, precision, and uncertainty. The monitoring was performed for 110 samples such as glass cups, containers, pots, and bottles. a food simulant. Migration test was conducted at 25? for 24 hours in a dark place using 4% acetic acid as a food simulant. Based on the data; exposure assessment was carried out to compare the estimated daily intake (EDI) to the human safety criteria. The risk levels of Pb and Ba determined in this study were approximately 1.9% and 0.3% of the provisional tolerable weekly intake (PTWI) and tolerable daily intake (TDI) value, respectively, thereby indicating a low exposure to the population.

Objective and Relative Sweetness Measurement by Electronic-Tongue (전자혀를 이용한 객관적 상대 단맛 측정)

  • Park, So Yeon;Na, Sun Young;Oh, Chang-Hwan
    • The Journal of the Convergence on Culture Technology
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    • v.8 no.6
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    • pp.921-926
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    • 2022
  • Sugar solutions (5%, 10%, 15% and 20%) were tested by seven sensors of Astree E-Tongue for selecting a sensor for sweetness. NMS sensor was chosen as a sensor for sweetness among two sensors (PKS and NMS sensors selected in first stage) by considering precision, linearity and accuracy. Sugar, fructose, glucose and xylitol (5%, 10% and 15%) were tested by E-tongue. The principal component analysis (PCA) result by E-Tongue with seven sensors at 5% concentration level of four sweetners was not satisfactory (Discrimination index was -0.1). On the other hand, the relative NMS sensor response values were derived as 1.08 (fructose), 0.99 (glucose) and 1.00 (xylitol) comparing to sugar. Only the E-Tongue relative glucose response 0.99 was different from 0.5~0.75 of the relative sweetness range reported as the human sensory test results. Considering the excellent precision (%RSD, 1.53~3.64%) of E-Tongue using NMS single sensor for three types of sweeteners compared to sugar in the concentration range of 5% to 15%, replacing sensory test of sweetened beverages by E-Tongue might be possible for new product development and quality control.

Estimation of Non-linear Strength and Stiffness for Silty Sands (실트질 모래지반의 비선형 강도 및 강성도 추정법)

  • Lee Kyung-Sook;Kim Hyun-Ju;Lee Jun-Hwan
    • Journal of the Korean Geotechnical Society
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    • v.22 no.1
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    • pp.35-44
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    • 2006
  • In general typically granular soils contain a certain amount of fines. It is also widely recognized that foundation soils under working loads show highly non-linear behavior from very early stages of loading. In the present study, a series of laboratory tests with sands of different silt contents are conducted and methods to assess strength and stiffiness characteristics are proposed. Modified hyperbolic stress-strain model is used to analyze non-linearity of silty sands in terms of non-linear Degradation parameters f and g as a function of silt contents and Relative density Dr. Stress-strain curves were obtained from a series of triaxial tests on sands containing different amounts of silt. Initial shear modulus, which is used to normalize Degradation modulus of silty sands, was determined from resonant column test results. From the laboratory test results, it was observed that, as the Relative density increases, values of f decrease and those of g increase. In addition, it was found that values of f and g increase and decrease respectively as a Skeleton void ratio $(e_{sk})$ increases.

Bioequivalence of pioglitazone tablet to Actos® tablet (Pioglitazone 30 mg) (액토스정®(피오글리타존 30 mg)에 대한 염산피오글리타존정의 생물학적동등성)

  • Yeom, Hyesun;Lee, Tae Ho;Youm, Jeong-Rok;Song, Jin-Ho;Han, Sang Beom
    • Analytical Science and Technology
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    • v.22 no.1
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    • pp.101-108
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    • 2009
  • The bioequivalence of two pioglitazone tablets, Actos$^{(R)}$ tablet (Takeda Chemical Industries, reference drug) and Pioglitazone tablet (Boryung Company, test drug) was evaluated according to the guidelines of Korea Food and Drug Administration. Twenty-eight healthy male Korean volunteers received each medicine (pioglitazone dose of 30 mg) in a $2{\times}2$ crossover study with one week washout interval. After drug administration, blood samples were collected at specific time intervals from 0-36 hours. The plasma concentrations of pioglitazone were determined by high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). The total chromatographic run time was 5 min and calibration curves were linear over the concentration range of 5-2000 ng/mL for pioglitazone. The method was validated for selectivity, sensitivity, linearity, accuracy and precision. The pharmacokinetic parameters were determined from the plasma concentration-time profiles of both formulations. The primary calculated pharmacokinetic parameters were compared statistically to evaluate bioequivalence between the two preparations. The 90% confidence intervals of the $AUC_t$ ratio and the $C_{max}$ ratio for Pioglitazone tablet and Actos$^{(R)}$ tablet were log0.9422~log1.1040 and log0.9200~log1.1556, respectively. Based on the statistical considerations, we can conclude that the test drug, Pioglitazone tablet was bioequivalent to the reference drug, Actos$^{(R)}$ tablet.

Establishment of Biotin Analysis by LC-MS/MS Method in Infant Milk Formulas (LC-MS/MS를 이용한 조제유류 중 비오틴 함량 분석법 연구)

  • Shin, Yong Woon;Lee, Hwa Jung;Ham, Hyeon Suk;Shin, Sung Cheol;Kang, Yoon Jung;Hwang, Kyung Mi;Kwon, Yong Kwan;Seo, Il Won;Oh, Jae Myoung;Koo, Yong Eui
    • Journal of Food Hygiene and Safety
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    • v.31 no.5
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    • pp.327-334
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    • 2016
  • This study was conducted to establish the standard method for the contents of biotin in milk formulas. To optimize the method, we compared several conditions for liquid extraction, purification and instrumental measurement using spiked samples and certified reference material (NIST SRM 1849a) as test materials. LC-MS/MS method for biotin was established using $C_{18}$ column and binary gradient 0.1% formic acid/acetonitrile, 0.1% formic acid/water mobile phase is applied for biotin. Product-ion traces at m/z 245.1 ${\rightarrow}$ 227.1, 166.1 are used for quantitative analysis of biotin. The linearity was over $R^2=0.999$ in range of $5{\sim}60{\mu}g/L$. For purification, chloroform was used as a solvent for eliminating lipids in milk formula. The linearity was over 0.999 in range of 5~60 ng/mL. The detection limit and quantification limit were 0.10, 0.31 ng/mL. The accuracy and precision of LC-MS/MS method using CRM were 103%, 2.5% respectively. Optimized methods were applied in sample analysis to verify the reliability. All the tested milk formulas were acceptable contents of biotin compared with component specification and standards for nutrition labeling. The standard operating procedures were prepared for biotin to provide experimental information and to strengthen the management of nutrient in milk formula.

Simultaneous Determination of Water Soluble Vitamins B Group in Health Functional Foods etc. by HPLC (건강기능식품 등 중 수용성 비타민 B군의 HPLC를 이용한 동시분석법)

  • Kim, Seon Hee;Kim, Jae-Hyun;Lee, Hwa Jung;Oh, Jae Myoung;Lee, Sung Hye;Bahn, Kyeong Nyeo;Seo, Il Won;Lee, Young Joo;Lee, Jin Hee;Kang, Tae Seok
    • Journal of Food Hygiene and Safety
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    • v.30 no.2
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    • pp.143-149
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    • 2015
  • This study was conducted to simultaneous analysis methods for water soluble vitamins B group (vitamin $B_1$, vitamin $B_2$, nicotinic acid, nicotinamide, vitamin $B_6$) which is used as health functional foods etc. Analytical methods of water-soluble vitamins B group by HPLC were established through instrumental analytical conditions, and the examination of data such as domestic and foreign reliable methods, and papers of journal. HPLC method analyzing water soluble vitamins B group was established using Capcell Pak C18 UG 120 column in 270 nm through test of columns. The validation has been performed on the method to determine linearity, accuracy, limits of quantification (LOQ) and repeatability for water soluble vitamins B group. An excellent linearity ($r^2=0.999$) was observed for vitamin $B_1$, vitamin $B_2$, nicotinic acid, nicotinamide, vitamin $B_6$ in the concentration range ($0.1{\sim}2{\mu}g/mL$). Observed recovery of vitamin $B_1$ was found to be between 100 and 103%, vitamin $B^2$ was found to be between 104 and 112%, nicotinic acid was found to be between 82 and 85%, nicotinamide was found to be between 121 and 124% and vitamin $B_6$ was found to be between 95 and 104%. LOQ of vitamin $B_1$ was found to be $0.04{\mu}g/mL$, vitamin $B_2$ was found to be $0.05{\mu}g/mL$, nicotinic acid was found to be $0.15{\mu}g/mL$, nicotinamide was found to be $0.08{\mu}g/mL$ and vitamin $B_6$ was found to be $0.63{\mu}g/mL$. Repeatability precision for vitamin $B_1$ was found to be 0.4%, vitamin $B_2$ was found to be 0.4%, nicotinic acid was found to be 0.5%, nicotinamide was found to be 0.7% and vitamin $B_6$ was found to be 0.4% relative standard deviation (RSD). Also, verify the accuracy of the simultaneous analysis methods, we monitored the labeled contents of the health functional foods and children's preferred foods.

Establishment of Choline Analysis in Infant Formulas and Follow-up Formulas by Ion Chromatograph (이온크로마토그래프를 이용한 조제유류 및 영아용·성장기용 조제식 중 콜린 함량 분석법 연구)

  • Hwang, Kyung Mi;Ham, Hyeon Suk;Lee, Hwa Jung;Kang, Yoon Jung;Yoon, Hae Seong;Hong, Jin Hwan;Lee, Hyoun Young;Kim, Cheon Hoe;Oh, Keum Soon
    • Journal of Food Hygiene and Safety
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    • v.32 no.5
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    • pp.411-417
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    • 2017
  • This study was conducted to establish the analysis method for the contents of choline in infant formulas and follow-up formulas by ion chromatograph (IC). To optimize the method, we compared several conditions for extraction, purification and instrumental measurement using spiked samples and certified reference material (CRM; NIST SRM 1849a) as test materials. IC method for choline was established using Ion Pac CG column and 18 mM $H_2SO_4$ mobile phase. The parameters of validation were specificity, linearity, LOD, LOQ, recovery, accuracy, precision and repeatability. The specificity was confirmed by the retention time and the linearity, $R_2$ was over 0.999 in range of 0.5~10 mg/L. The detection limit and quantification limit were 0.14, 0.43 mg/L. The accuracy and precision of this method using CRM were 95%, 2.1% respectively. Optimized methods were applied in sample analysis to verify the reliability. All the tested products were acceptable contents of choline compared with component specification for nutrition labeling. The standard operating procedures were prepared for choline to provide experimental information and to strengthen the management of nutrient in infant formula and follow-up formula.