• Title/Summary/Keyword: linearity test

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A Study on the Possibility of Using Fire-Retardant Working Cloth Made from Silicon Carbide (SiC) Composite Spun Yarns (Silicon Carbide (SiC) 복합방적사로부터 제조된 원단의 방화복 활용 가능성에 관한 연구)

  • Kang, Hyun-Ju;Kang, Gun-Woong;Kwon, Oh-Hoon;Kwon, Hyeon-Myoung;Hwang, Ye-Eun;Jeon, Hye-Ji;Joo, Jong-Hyun;Park, Yong-Wan
    • Science of Emotion and Sensibility
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    • v.24 no.4
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    • pp.149-156
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    • 2021
  • The mechanical properties of a woven fabric made of SiC (silicon carbide) fibers were determined in this study using the KES-FB system. The woven fabric is used in high heat settings above 1500℃. Composite spun yarns were used to create SiC fibers. By analyzing the wearing properties, we studied the prospect of using the textiles as fire-retardant work clothes. Mechanical properties determine the wearing attributes. Therefore, the tensile linearity (LT), tensile resilience (RT), and shear stiffness (G) values of the fabric varied according to the yarn type (filament or spun yarn). The thickness, weight per square meter, and density of the fabric were found to have an effect on the shear hysteresis (2HG) and compression resilience (RC) values. In terms of wearable clothing qualities, the fabric qualities of the SiC composite yarn demonstrated the highest ratio of compressive energy to thickness (WC/T), which indicates bulkiness. The fabric manufactured from SiC composite yarns passed the KFI criteria for carbonation length and cumulative flame time in the flame-retardant test. Therefore, we discovered that the material can be used as a fire-resistant work cloth.

Development of LC-MS/MS analytical methods for metalaxyl in Atractylodes macrocephala Koidzumi and Achyranthes japonica Nakai (LC-MS/MS를 이용한 생약 백출 및 우슬 중 Metalaxyl 잔류분석법 개발)

  • Yun, Myung-Sub;Yang, Seung-Hyun;Choi, Hoon
    • Journal of Applied Biological Chemistry
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    • v.65 no.1
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    • pp.17-21
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    • 2022
  • A new rapid and simple method for metalaxyl in Atractylodes macrocephala Koidzumi and Achyranthes japonica Nakai has been developed and validated. This study was conducted to develop a method for analyzing metalaxyl by a method based on QuEChERS using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Samples were extracted with acetonitrile and purified using amino-propyl (NH2) Solid Phase Extraction cartridge. The method limit of quantitation (MLOQ) was 0.01 mg/kg. The linearity of matrix-matched calibration curve (r2) was ≥0.99 at the calibration range of 0.001-0.05 mg/kg. For recovery test, Atractylodes macrocephala Koidzumi or Achyranthes japonica Nakai was treated with standard solutions at MLOQ and 10MLOQ levels. Recovery rates were in the range of 88.1-109.1% with <5.5% coefficient of variation. This established analytical method was fully validated. Based on these results, it can contribute to improving the safety of residual pesticides in Atractylodes macrocephala Koidzumi and Achyranthes japonica Nakai.

Optimization of Analytical Methods for Octacosanol in Related Health-functional Foods with GC-MS (GC-MS를 이용한 건강기능식품 중 옥타코사놀 분석법 개발 연구)

  • Lee, Jin Hee;Oh, Mi Hyune;Lee, Kyung Jin;Kim, Yang Sun;Keum, Eun Hee;Park, Ji Eun;Cho, Mee Hyun;Seong, Min Hye;Kim, Sang A;Kim, Mee hye
    • Journal of Food Hygiene and Safety
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    • v.33 no.4
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    • pp.266-271
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    • 2018
  • The Ministry of Food and Drug Safety (MFDS) is amending its test methods for health-functional foods (dietary food supplements) to establish regulatory standards and specifications in Korea. In this regard, we continue our research on developing analytical methods for the items. Octacosanol is the major component of polycosanol and is a high-molecular-mass primary fatty alcohol, obtained from sugar cane wax. Previous researchers have shown that octacosanol can lower cholesterol and has antiaggregatory properties, cytoprotective uses, and ergogenic properties for human health. Recently, octacosanol products have been actively introduced into the domestic market because of their functional biological activity. We have developed a sensitive and selective test method for octacosanol that the TMS derivatives by means of gas-chromatographic-tandem mass spectrometry (GC-MS). The trimethylsilyl ether derivative of the target analyte showed excellent chromatographic properties. The procedure was validated in the range of $12.5{\sim}200{\mu}g/L$. Standard calibration curves presented linearity with the correlation coefficient ($r^2$) > 0.999, and the limits of detection (LOD) and limits of quantitation (LOQ) were $4.5{\mu}g/L$ and $13.8{\mu}g/L$, respectively. The high recoveries (92.5 to 108.8%) and precision (1.8 to 2.4%) obtained are in accordance with the established validation criteria. Our research can provide scientific evidence to amend the octacosanol test method for the Health-Functional Food Code.

Method Development of Ellagic Acid as Marker Compound for Standardization of Gochang Bokbunja (Rubus coreanus Miquel) as Functional Ingredient (고창 복분자의 기능성원료 표준화를 위한 지표성분으로서 Ellagic Acid의 분석법 개발)

  • Kim, Yunjeong;Han, Song-Hee;Jeon, Ji-Yeong;Hwang, Minho;Im, Yong-Jin;Chae, Soo-Wan;Kim, Min-Gul
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.41 no.11
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    • pp.1554-1558
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    • 2012
  • Method development and validation of ellagic acid for the standardization of Gochang Bokbunja as a functional ingredient and health food were accomplished. A Symmetry$^{(R)}$ (C18, $4.6{\times}250mm$, $5.0{\mu}m$) column was used with a gradient elution system of 1% formic acid in water and acetonitrile. This method was validated according to specificity, linearity, accuracy, precision test, and recovery test. Specificity was confirmed with identical retention time, and calibration curves of ellagic acid showed good linear regression ($R^2$ >0.9996). Relative standard deviations (RSD) of data from the intra- and inter-day experiments were less than 2.28% and 2.84%, except in the low limit of quality control (LLOQ, $1{\mu}g/mL$) sample. The results of the recovery test were from 89.17% to 97.92% with RSD values from 0.05 to 0.14%. Therefore, we performed analysis of ellagic acid as a marker compound in Gochang Bokbunja extracts. The amount of ellagic acid in Gochang Bukbunja was about $1.918{\mu}g/mg$ (0.192%) in the three times analysis, and RSD was less than 2.36% by the validated method. These results suggest that the developed HPLC method is simple, efficient, and could contribute to the quality control of Gochang Bokbunja extract as a functional ingredient.

Harmonization of Hemolysis Index in Clinical Chemistry Laboratory and Its Application as a Result Verification Tool (화학검사 결과의 검증을 위한 용혈 지수 일치화 도구 개발)

  • Pyo, Sang Shin;Nam, Hyun Su;Cha, Young Jong;Lee, Seungkwan;Lee, Hae Kyung
    • Korean Journal of Clinical Laboratory Science
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    • v.49 no.4
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    • pp.350-358
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    • 2017
  • The hemolysis index (HI) is semi-quantitative marker for hemolysis. Because the characteristics of the HI vary from one commercial platform to another, no standardization or harmonization of the HI is currently available. Specimens (N=40) randomly selected from clinical patients were artificially hemolyzed in vitro. The serum of the specimens was then diluted with a 20 mg/dL difference between 0~300 mg/dL based on serum hemoglobin measured using the XE-2100 hematology automation equipment (Sysmex, Japan). Diluted serum was measured using the Hitachi-7600 biochemical automation equipment (Hitachi, Japan) to differentiate between HI and serum hemoglobin. The data showed linearity between HI and serum hemoglobin and that HI 1 contained approximately 20 mg/dL of serum hemoglobin. To determine the blood rejection threshold, the HI was divided into three groups: HI 0~1, HI 4~6, HI 9~15. After another batch of clinical specimens (N=40) was measured using a Hitachi-7600 (Hitachi, Japan), each specimen was moved forward and backward with the piston of the syringe to induce an artificial in vitro hemolysis, then measured again with a Hitachi-7600 (Hitachi, Japan). The percentage difference between the three groups was analyzed by ANOVA or the Kruskal-Wallis test. In the post-test, there were significant differences between the HI 0~1 and the HI 5~6: Glucose, creatinine, total protein, AST, direct bilirubin, uric acid, phosphorus, triglyceride, LDH, CPK, Magnesium, and potassium levels. Because many clinical tests differed significantly, the threshold for hemolysis could be appropriate for HI 5 (serum hemoglobin 100 mg/dL).

Analytical Method Development for Determination of Silymarin by LC-MS/MS for Related Health Functional Foods (LC-MS/MS를 이용한 건강기능식품 중 실리마린 분석법 연구)

  • Oh, Mihyune;Lee, Jin Hee;Kim, Sang-A;Kim, Meehye
    • Journal of Food Hygiene and Safety
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    • v.33 no.2
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    • pp.124-130
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    • 2018
  • The Ministry of Food and Drug Safety (MFDS) is amending its test methods for the use of health functional foods (dietary food supplement), in order to establish regulatory standards and specifications in Korea. In this regard, we continue to pursue and perform our research on the analytical method development for the items being researched and reviewed. In this study, we have developed a sensitive and selective test method that could simultaneously separate and determinate six major bioactive flavonolignans in silymarin, which are based on the use of a liquid chromatographic-tandem mass spectrometry (LC-MS/MS). The standard calibration curves presented a linearity effect with the correlation coefficient ($r^2$) > 0.999. The limits of detection (LODs) and limits of quantitation (LOQs) were in the range of $0.3{\sim}9.0{\mu}g/L$ and $0.8{\sim}27.3{\mu}g/L$, respectively. The recovery results ranged between 96.2~98.6% at 3 different concentration levels, and its relative standard deviations (RSDs) were less than 5% as noted in this study. The proposed analytical method was characterized with a noted high resolution of the individual silymarin constituents, and the assay was fully validated as well. Our research can provide a significant scientific evidence that can be useful to amend the silymarin test method for the Health Functional Food Code.

Evaluation for Application of IOM Sampler for Agricultural Farmer's Inhalation Exposure to Kresoxim-methyl and Fenthion (농작업자의 Kresoxim-methyl과 fenthion에 대한 호흡노출량 측정을 위한 IOM 채집기의 효율성 평가)

  • Lee, Jiho;Kim, Eunhye;Lee, Jonghwa;Shin, Yongho;Maasfeld, Wolfgang;Choi, Hoon;Moon, Joon-Kwan;Lee, Hyeri;Kim, Jeong-Han
    • The Korean Journal of Pesticide Science
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    • v.19 no.3
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    • pp.230-240
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    • 2015
  • An IOM sampler equipped with glass fiber filter has been recently utilized instead of solid adsorbent, which was used to measure the inhalation exposure of agricultural operator to pesticides. The aim of this study is to validate the efficacy of an IOM sampler by measuring the trapping efficiency and breakthrough using kresoxim-methyl water-dispersible granule and fenthion emulsifiable concentrate. On LC-MS/ MS, minimum detection level was 12.5 pg and method limit of detection was 5.0 ng/mL. Good linearity ($R^2$ > 0.999) for matrix matched standards was obtained. Recoveries of pesticides from glass fiber filter were 102-109% (kresoxim-methyl) and 97-104% (fenthion) while those from XAD-2 resin were 94-98% (kresoxim methyl) and 93-100% (fenthion). Trapping efficiency test was performed with personal air pumps and IOM sampler (glass fiber filter) connected with solid adsorbent (XAD-2 resin) with two types of formulation (solid and liquid) which were diluted by standard rate and sprayed to IOM sampler. Those pesticides were trapped only in glass fiber filter without any breakthrough to solid adsorbent. After spiking of pesticides to glass fiber filter, breakthrough test was carried out with IOM sampler (glass fiber filter) which was connected with solid adsorbent. As a results, 87-101% of kresoxim-methyl and 96-105% of fenthion remained in spiked glass fiber filter, however, no pesticides were detected in second glass fiber filter and solid adsorbent. In conclusion, IOM sampler which equipped with glass fiber filter can be applied widely for pesticide inhalation exposure study since it has good trapping efficiency and adsorption capacity, regardless of the solid or liquid formulation.

Formaldehyde Monitoring of Hygiene Products in Domestic Market (국내 유통 위생용품 중 포름알데히드 잔류량 모니터링)

  • Na, Young-Ran;Kwon, Hyeon-Jeong;Cho, Hyun-Nho;Kim, Hyeon-Jin;Park, Yon-Koung;Park, Sung-Ah;Lee, Seong-Ju;Kang, Jung-Mi
    • Journal of Food Hygiene and Safety
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    • v.35 no.3
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    • pp.225-233
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    • 2020
  • By the standards and specifications for hygiene products, three test methods for formaldehyde are specified for each item type of hygiene product. After derivatization using acetylacetone and 2,4-dinitrophenylhydrazine (2,4-DNPH), formaldehyde is analyzed by spectrophotometer and high-performance liquid chromatography (HPLC). Validation of the three test methods was performed on tissue, diaper lining and waterproof layer, and panty liner products. The results of linearity (R2), limit of detection (LOD), limit of quantification (LOQ), recovery rate (%) and reproducibility (%), showed that all three methods are suitable for analyzing formaldehyde in hygiene products. After derivatization with 2,4-DNPH and cetylacetone, formaldehyde was analyzed at 0, 3, 6, 9, 24 and 48 hours by HPLC. Formaldehyde derivatized with 2,4-DNPH showed no statistically significant change in formaldehyde peak area over time (P>0.05). But, acetylacetone-derivatizated formaldehyde showed a negative correlation coefficient (r) over time (P<0.01). We investigated the residual amounts of formaldehyde in 205 hygiene products distributed in Busan. Among 74 disposable diaper products tested, 73 had low concentrations of formaldehyde (0.13-29.87 mg/kg). Moreover, formaldehyde was not detected in any of 78 tissue, 27 disposable paper towel, 12 disposable dishcloth, 7 paper cup, one brand of paper straw and 6 disposable napkin products.

Analysis of Diflubenzuron in Agricultural Commodities by Multiresidue Method (동시 다성분 분석법에 의한 농산물 중 Diflubenzuron 분석)

  • Park, Sun-Hee;Han, Chang-Ho;Kim, Ae-Kyung;Shin, Jae-Min;Lee, Jae-Kyoo;Park, Young-Hae;Kim, Ji-Min;Hwang, Lae-Hong;Chang, Min-Su;Song, Mi-Ok;Park, Ju-Sung;Yun, Eun-Sun;Kim, Mu-Sang;Jung, Kweon
    • The Korean Journal of Pesticide Science
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    • v.18 no.4
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    • pp.269-277
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    • 2014
  • The multiclass pesticide multiresidue method for the simultaneous determination of diflubenzuron in agricultural products was conducted by using HPLC-UVD. The method was validated through the guidelines of linearity, specificity, limit of detection (LOD), limit of quantification (LOQ), accuracy and precision with pesticide-free spinach, Korean cabbage, eggplant, squash, sweet pepper, cucumber, Korean melon. The calibration curve of diflubenzuron was linear over the concentration range of 0.05-5 mg/kg with correlation coefficient of above 0.99999. The limit of detection and quantification was 0.008 and 0.02 mg/kg. Mean recoveries of diflubenzuron for each sample were 77.5-105.6%. Relative standard deviation (RSD) in recoveries were all less than 20%. The intra-day and inter-day precision (RSD) were 0.4-1.9% and 0.7-1.9%, respectively. The result of validation indicated that this method was accurate and rapid assay.

Simultaneous Analysis for Veterinary Drug Residues in Honey by HPLC/MS/MS (HPLC-MS/MS를 이용한 벌꿀 중 동물용의약품 동시분석방법 연구)

  • Kim, Jong-Hwa;Moon, Sun-Ea;Kim, Ki-Yu;Jung, You-Jung;Lee, Chang-Hee;Ku, Eun-Jung;Yoon, Mi-Hye;Lee, Jong-Bok
    • Journal of Food Hygiene and Safety
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    • v.31 no.2
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    • pp.94-98
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    • 2016
  • This study was conducted to establish the simultaneous analysis method for veterinary drug residues in honey by high performance liquid chromatography tandem mass spectrometry (HPLC/MS/MS). The eleven targeting veterinary drugs with honey test method in Korean Food Standards Codex were divided into Group 1 (streptomycine dihydrostreptomycine, neomycine) and Group 2 (oxytetracycline, enrofloxacin, ciprofloxacin, cymiazole, chloramphenicol, amitraz, coumaphos, fluvalinate) to be analyzed simultaneously. From the results, the retention time (RT) of the targeting drugs was within 15 min, the range of detection limits was 0.0056 to $0.0643{\mu}g/g$ and the range of quantification limits was 0.0169 to $0.1948{\mu}g/g$. The coefficients of determination ($R^2$) for Group 1 ($0.05{\sim}1.0{\mu}g/mL$) and Group 2 ($0.01{\sim}1.0{\mu}g/mL$) were 0.9917~0.9987 and 0.9923~1.000 respectively, and showed the good linearity. The recovery rates for Group 1 (final conc. $0.25{\mu}g/g$) and Group 2 (final conc. $1.0{\mu}g/g$) were 65.1~80.6% and 64.2~90.3% respectively. Also, the analysis results of inter day (n = 3) and intra day (n = 6) RSD (%) for area and retention time showed that the RSD (%) for area and retention time was below 10.92% and 1.57%. Therefore, the simultaneous analysis method of this study is evaluated to be a good test method for veterinary drug residues in honey.