• Title/Summary/Keyword: Limit of determination

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Establishment of an Analytical Method for Novobiocin in Livestock Products Using HPLC-UVD (HPLC-UVD를 이용한 축산식품 중 Novobiocin의 시험법 확립)

  • Park, Hee-Ra;Kwon, Chan-Hyeok;Lee, Jong-Goo;Kim, Hyung-Soo;Chae, Young-Sik;Oh, Jae-Ho;Kwon, Ki-Sung
    • Korean Journal of Food Science and Technology
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    • v.44 no.3
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    • pp.263-268
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    • 2012
  • Novobiocin is a coumarin-containing antibiotic, and has a longer half-life in various animals than other veterinary medicines. A simple and rapid high-performance liquid chromatography assay for the determination of residual novobiocin levels in chicken, beef and milk has been developed and validated. The separation condition for HPLC/UVD was optimized by a MG II $C_{18}$ (4.6 mm $ID{\times}250$ mm, 5 ${\mu}m$) column with 0.1% formic acid in $H_2O$/0.1% formic acid in Acetonitrile (40/60, v/v) as the mobile phase at a flow rate of 1.0 mL/min and the detection wavelength was set at 340 nm. Residues were extracted from tissue by blending with methanol. After liquid-liquid partitioning, lipid materials were removed with n-hexane and purification as Silica (1 g, 6 mL) cartridge with 10 mL acetone/dichloromethane (10/90, v/v). Limit of quantification and linearity performed by the analytical method were 0.02 mg/kg and 0.999 ($r^2$), and the recovery range was $88.8{\pm}5.6-100.3{\pm}4.4$, $88.8{\pm}7.2-97.0{\pm}3.2$ and $88.1{\pm}4.3-92.8{\pm}3.6%$. It is expected that this analytical method with regards to novobiocin in chicken, beef and milk could be applied as an official method to administer food safety on veterinary medicines.

Development of Analysis Method of Caffeine and Content Survey in Commercial Foods by HPLC (HPLC를 이용한 카페인의 분석법 개발 및 시판 식품중 함유량 조사)

  • Kim, Hee-Yun;Lee, Young-Ja;Hong, Ki-Hyoung;Lee, Chul-Won;Kim, Kil-Saeng;Ha, Sang-Chul
    • Korean Journal of Food Science and Technology
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    • v.31 no.6
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    • pp.1471-1476
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    • 1999
  • A simple and practical method for determination of caffeine in foods was developed. The analysis of caffeine was performed by reverse phase high performance liquid chromatography using a ${\mu}-Bondapak\;C_{18}$ column at isocratic condition with methanol-acetic acid-water(20 : 1 : 79) on UV detector at 280 nm. The clean-up and extraction of caffeine in samples were based on a simple pretreatment using a Sep-Pak $C_{18}$ cartridge. Recovery rates obtained with this method for cider, candy, cookie, milk, ice cream and persimmon leaf tea were 99.23%, 99.50%, 99.17%, 99.37%, 98.93% and 99.10% respectively. And the detection limit of caffeine was $0.1\;{\mu}g/mL$. With this method, the range of caffeine contents extracted from coffee, green tea, black tea, Oolong tea(tea bag), soft drinks, ice cream, milk and commercial confectionery were $3.38{\sim}37.50\;mg/g,\;16.30{\sim}26.10\;mg/g,\;10.80{\sim}16.65\;mg/g,\;11.25\;mg/g,\;0.06{\sim}0.11\;mg/g,\;0.04{\sim}0.44\;mg/g,\;0.04{\sim}0.39\;mg/g\;and\;0.10{\sim}1.80\;mg/g$, respectively. But caffeine was not detected in the other tea such as Acanthopanax sessiliflorum tea, Angelica gigas tea, Angelica tea, Arrow root tea, Duchu'ng tea, Dunggulle tea, Ganoerma lucidum tea, Ginger tea powder, Persimmon leaf tea, Ssanghwa tea and Cocoa mix powder.

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Method Validation and Quantification of Lutein and Zeaxanthin from Green Leafy Vegetables using the UPLC System (UPLC를 이용한 lutein과 zeaxanthin의 분석법 검증 및 엽채류에서의 정량적 평가)

  • Kim, Suna;Kim, Ji-Sun
    • Korean Journal of Food Science and Technology
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    • v.44 no.6
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    • pp.686-691
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    • 2012
  • The objective of this research is to present method development and validation for the simultaneous determination of lutein and zeaxanthin using ultra performance liquid chromatography (UPLC). Also, rapid quantification was performed on six green leafy vegetables (Allium tuberosum, Aster scaber, Hemerocallis fulva, Pimpinella brachycarpa, Sedum sarmentosum and Spinacia oleracea) that are commonly consumed in Korea. Separation and quantification were successfully achieved with a Waters Acquity BEH C18 ($50{\times}2.1mm$, $1.7{\mu}m$) column by 85% methanol within 5 min. Two compounds showed good linearity ($r^2$ > 0.9968) in $1-150{\mu}g/mL$. Limit of detection (LOD) and quantification (LOQ) for lutein and zeaxanthin were 1.7 and 5.1 g/mL and 2.1 and 6.3 g/mL, respectively. The RSD for intra- and inter-day precision of each compound was less than 10.69%. The recovery of each compound was in the range of 91.75-105.13%. Aster scaber and Spinacia oleracea contained significantly higher amounts of lutein ($4.06{\pm}0.24$ and $3.97{\pm}0.10mg$/100 g of fresh weight), respectively.

Simultaneous determination of 11-nor-Δ9-carboxy-tetrahydrocannabinol and 11-nor-Δ9-carboxy-tetrahydrocannabinol-glucuronide in urine samples by LC-MS/MS and its application to forensic science (LC-MS/MS를 이용한 소변 중 11-nor-Δ9-carboxy-tetrahydrocannabinol 및 11-nor-Δ9-carboxy-tetrahydrocannabinol-glucuronide의 동시 분석 및 법과학적 적용)

  • Park, Meejung;Kim, Sineun
    • Analytical Science and Technology
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    • v.34 no.6
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    • pp.259-266
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    • 2021
  • Cannabis (Marijuana) is one of the most widely used drugs in the world, and its distribution has been controlled in South Korea since 1976. Identification of 11-nor-Δ9-carboxy-tetrahydrocannabinol (THCCOOH) in urine can provide important proof of cannabis use, and it is considered scientific evidence in the forensic field. In this study, we describe a simultaneous quantitative method for identifying THCCOOH and THCCOOH-glucuronide in urine, using simple liquid-liquid extraction (LLE), and liquid chromatography-tandem mass spectrometry (LC-MS/MS). THCCOOH-D3 and THCCOOH-glucuronide-D3 were used as internal standards. Validation results of the matrix effect, as well as recovery, linearity, precision, accuracy, process efficiency, and stability were all satisfactory. No carryover, endogenous or exogenous interferences were observed. The limit of detection (LOD) of THCCOOH and THCCOOH-glucuronide were 0.3 and 0.2 ng/mL, respectively. The developed method was applied to 28 authentic human urine samples that tested positive in immunoassay screening and gas chromatography/mass spectrometry (GC/MS) tests. The ranges of concentrations of THCCOOH and THCCOOH-glucuronide in the samples were less than LOQ~266.90 ng/mL and 6.43~2133.03 ng/mL, respectively. The concentrations of THCCOOH-glucuronide were higher than those of THCCOOH in all samples. This method can be effectively and successfully applied for the confirmation of cannabinoid use in human urine samples in the forensic field.

A Study on LRFD Reliability Based Design Criteria of RC Flexural Members (R.C. 휨부재(部材)의 L.R.F.D. 신뢰성(信賴性) 설계기준(設計基準)에 관한 연구(研究))

  • Cho, Hyo Nam
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.1 no.1
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    • pp.21-32
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    • 1981
  • Recent trends in design standards development in some European countries and U.S.A. have encouraged the use of probabilistic limit sate design concepts. Reliability based design criteria such as LSD, LRFD, PBLSD, adopted in those advanced countries have the potentials that they afford for symplifying the design process and placing it on a consistent reliability bases for various construction materials. A reliability based design criteria for RC flexural members are proposed in this study. Lind-Hasofer's invariant second-moment reliability theory is used in the derivation of an algorithmic reliability analysis method as well as an iterative determination of load and resistance factors. In addition, Cornell's Mean First-Order Second Moment Method is employed as a practical tool for the approximate reliability analysis and the derivation of design criteria. Uncertainty measures for flexural resistance and load effects are based on the Ellingwood's approach for the evaluation of uncertainties of loads and resistances. The implied relative safety levels of RC flexural members designed by the strength design provisions of the current standard code were evaluated using the second moment reliability analysis method proposed in this study. And then, resistance and load factors corresponding to the target reliability index(${\beta}=4$) which is considered to be appropriate level of reliability considering our practices are calculated by using the proposed methods. These reliability based factors were compared to those specified by our current ultimate strength design provisions. It was found that the reliability levels of flexural members designed by current code are not appropriate, and the code specified resistance and load factors were considerably different from the reliability based resistance and load factors proposed in this study.

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Study on the determination methods of the natural radionuclides (238U, 232Th) in building materials and processed living products (실내 건축자재 및 생활 가공제품 중 천연방사성핵종(238U, 232Th)의 농도 평가를 위한 분석법 연구)

  • Lee, Hyeon-Woo;Lim, Jong-Myoung;Lee, Hoon;Park, Ji-Young;Jang, Mee;Lee, Jin-Hong
    • Analytical Science and Technology
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    • v.31 no.4
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    • pp.149-160
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    • 2018
  • A large number of functional living products are being produced for eco-friendly or health-promoting purposes. In the manufacturing process, such products could be adulterated with raw materials with high radioactivity, such as monazite and tourmaline. Thus, it is essential to manage raw materials and products closely related to the public living. For proper management, an accurate radioactivity data of the processed products are needed. Therefore, it is essential to develop a rapid and validated analytical method. In this study, the concentration of the radioactive $^{238}U$ and $^{232}Th$ in building materials (e.g., tile, cement, paint, wall paper, and gypsum board) and living products (e.g., health products, textiles, and minerals) were determined and compared by ED-XRF and ICP-MS. By comparing the results of both methods, we confirmed the applicability of the rapid screening and precise analysis of ED-XRF and ICP-MS. In addition, $^{238}U$ and $^{232}Th$ levels were relatively lower in building materials than in living products. Particularly, $^{232}Th$ content in 6 of 47 living products exceeded (maximum $8.2Bq{\cdot}g^{-1}$) the standard limit of $^{232}Th$ content in raw material ($1.0Bq{\cdot}g^{-1}$).

An Assessment of Notice Exposure by Job and Dosimeter Parameters Setting in Automobile Press Factory (자동차 프레스 공정에 있어서 직무 및 누적소음기 설정치 차이에 따른 작업자의 소음노출 평가)

  • Jeong, Jee Yeon;Park, Seunghyun;Yi, GwangYong;Lee, Naroo;You, Ki Ho;Park, Junsun;Chung, Ho Keun
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.11 no.3
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    • pp.190-197
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    • 2001
  • Noise-induced hearing loss(NIHL) was the highest rate (43.5%~58.5% from 1996 to 1998) of positive findings through specific medical program in Korea. There were much more NIHL at workers of automobile manufacturing factories than other manufacturing factories. The specific aim of the present study was to determine the noise exposure of automobile press lines, according to their job titles, press line types(auto, semiauto), dosimeter parameters setting. There were a total 11 press lines sampled at a automobile manufacturing company. Among those press lines, 10 press lines were autolines with acoustic enclosure, one semiauto press line was no aucostic enclosure Noise exposure data were sampled for an work shift using noise dosimeter, which recorded both time-weighted average(TWA) and 1-min average. The mean OSHA TWA(Korea TWA with threshold 90) was $80.7dB(A){\pm}4.7dB(A)$ for leader, $82.8dB(A{\pm}4.5dB(A)$ for pallette man, $76.7dB(A){\pm}4.3dB(A)$ for press operators, $76.6dB(A){\pm}5.6dB(A)$ for crane operators, $77.1dB(A){\pm}2.8dB(A)$ for forklift drivers, whereas the mean NIOSH TWA was $88.9dB(A){\pm}1.7dB(A)$ for leader, $89.6dB(A){\pm}2.1dB(A)$ for pallette man, $86.7dB(A){\pm}1.8dB(A)$ for press operators, $88.5dB(A){\pm}2.0dB(A)$ for crane operators, $87.7dB(A){\pm}1.0dB(A)$ for forklift drivers. While L10 for NIOSH TWA samples was 84.8 dB(A) ~ 87.3 dB(A), L10 for OSHA TWA samples was 69.5 dB(A) ~ 77.4 dB(A). L10 means that the TWA for 90% of the samples exceeded L10. Among OSHA TWA(Korea TWA with threshold 90) samples for pallette man, 7.7 % exceeded 90 dB(A), the OSHA permissible exposure level, but OSHA TWA samples for the other job titles didn't. Among NIOSH TWA samples, the samples over 85 dB(A), the NIOSH recommended exposure limit, was 100% (leaders), 83.3 %(operators), 97.4%(palletteman), 100%(forklift drivers), 91.7 %(crane operator). The results of One-way random effects analysis of variance models shows that the difference between job titles was significant by OSHA TWA(p<0.05), but not significant by NIOSH TWA(p>0.05). NIOSH TWA samples were significantly higher than OSHA TWA samples(P<0.05). Regression analysis was used to obtain relationships between OSHA TWA samples and NIOSH TWA samples. In this case the coefficient of determination = 0.90, which shows the high degree association between two methods. Regression equation, NIOSH TWA = 0.552 * OSHA TWA + 42.13 dB(A), shows that if OSHA TWA is known, NIOSH TWA can be predicted by the equation. The mean TWA difference between threshold 80 dBA and 90 dBA was significant(p<0.01). While the TWA noise exposures were 7.7% above the Korea(OSHA) PEL, they were more than 83.3% over NIOSH REL. Automobile workers were exposed to noise level that could be potentially damaging to their hearing. It found that there is approximately 25% excess risk of hearing loss even if a worker is protected to the PEL in according to NIOSH study.

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Determination of Dithiocarbamates in Agricultural Products Circulated in Korea (시판 농산물의 dithiocarbamates 분석)

  • Kim, Hee-Yun;Choi, Hee-Ju;Eom, Ji-Yoon;Seo, Eun-Chae;Choi, Sung-Hee;Cheong, So-Young;Choi, Sun-Hee;Lee, Hwa-Jeong;Choi, Jae-Chun
    • Korean Journal of Food Science and Technology
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    • v.42 no.1
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    • pp.1-7
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    • 2010
  • To revise the dithiocarbamates residue analysis method and survey the residues in agricultural products that were treated with these fungicides in Korea, we purchased 20 types of foodstuffs (rice, potato, cabbage, apple etc.) from markets in five major cities. 236 samples of the purchased foodstuffs were then analyzed for the presence of dithiocarbamates by HPLC/UV and HPLC/APCI-MS. The $R^2$, LOD and LOQ in the range of 0.5-107.3 mg/L were as follows: DCC: y=174.34x+18.315, $R^2=0.9999$, 0.01 mg/L, and 0.04 mg/L; EBDC: y=227.38x-14.715, $R^2=1.0000$, 0.01 mg/L and 0.02 mg/L; PBDC: y=38.46x-21.412, $R^2=0.9999$, 0.04 mg/L, and 0.1 mg/L; ETU: y=52.752x-4.4819, $R^2=0.9998$, 0.02 mg/L and 0.03 mg/L; PTU: y=128.28x+4.4624, $R^2=0.9998$, 0.02 mg/L, and 0.04 mg/L. The levels of DDC, EBDC, PBDC, ETU and PTU in 20 agricultural products fortified to 10.0-107.3 mg/L ranged from 61.7-117.5%, 65.3-110.1%, 61.5-109.6%, 69.3-116.3% and 70.2-97.2%, respectively. Overall, dithiocarbamates were detected in 100 samples and the detection ratio was 42.4%. Among these, only 3 samples (1.3%) of Lycii fructus had residue levels that were above the action limits, while the remaining samples (233 samples) contained levels of dithiocarbamates below the detection limit or below the Korea MRLs (Maximum Residue Limits).