• Title/Summary/Keyword: LOD

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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.

Validation of a Method and Evaluation of Antioxidant Activity for the Simultaneous Determination of Riboflavin and Coixol in Coix lacryma-jobi var. ma-yuen Stapf Sprouts (율무 새싹 추출물의 Riboflavin과 Coixol의 동시 분석법 검증 및 항산화 활성)

  • Lee, Ji Yeon;Park, Jung Yong;Park, Chun-Geon;Kim, Dong Hwi;Ji, Yun-Jeong;Choi, Su Ji;Oh, MyeongWon;Hwang, Hosop;Lee, Yunji;Jeong, Jintae;Lee, Jeong Hoon;Seo, Kyung Hye
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.64 no.4
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    • pp.452-458
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    • 2019
  • Coix lacryma-jobi var. ma-yuen (Rom. Caill.) Stapf (CL), which contains riboflavin and coixol, has traditionally been used to treat cancer and arthritis. However, no method for the simultaneous determination of riboflavin and coixol in CL sprouts has been established. In this study, we established and validated a high-performance liquid chromatography-diode array detection (HPLC-DAD) method for the identification and quantification of two reference markers, riboflavin and coixol, in CL sprout extracts. CL sprouts (whole sprouts and leaves) were subjected to extraction with 70% ethanol at room temperature and at 80 ℃ under reflux conditions. The two extractions were validated with respect to specificity, accuracy, precision, and linearity. The content of the two reference markers was highest in leaves extracted under reflux conditions (riboflavin, 8.23 ± 0.32 mg/g; coixol, 5.95 ± 0.04 mg/g). We also investigated the antioxidant activity of the extracts via 2,2-diphenyl-1-picrylhydrazyl (DPPH) and 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS+) scavenging assays. The results indicated that extracts obtained from sprouts under reflux conditions had the strongest antioxidative effects (DPPH half maximal inhibitory concentration [IC50], 68.9 ± 4.1 g/mL; and ABTS, IC50, 34.9 ± 0.1 g/mL). These results can serve as baseline data for the simultaneous determination of the two reference marker compounds, riboflavin and coixol, and development of functional food materials using CL sprouts.

Residue Patterns of Indoxacarb and Thiamethoxam in Chinese Cabbage(Brassica campestris L.) Grown under Greenhouse Conditions and Their Estimated Daily Intake (비닐하우스 재배 얼갈이배추 중 Indoxacarb와 Thiamethoxam의 잔류특성 및 식이섭취량)

  • Lee, Eun-Young;Kim, Dae-Kyu;Park, In-Young;Noh, Hyun-Ho;Park, Young-Soon;Kim, Tae-Hwa;Jin, Chung-Woo;Kim, Kwang-Ill;Yun, Sang-Soon;Oh, Sang-Kyun;Kyung, Kee-Sung
    • Korean Journal of Environmental Agriculture
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    • v.27 no.1
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    • pp.92-98
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    • 2008
  • This experiment was carried out to investigate the residue patterns of two insecticides, indoxcarb and thiamethoxam, commonly used for Chinese cabbage, under greenhouse conditions. The pesticides were sprayed onto Chinese cabbage at the recommended dose and double of the recommended dose 10 days before the prearranged harvest and then sampling was done at 0.17, 1, 2, 3, 4, 5, 6, 8, 10, and 12 days after spraying. The amounts of their residues in the crop were analyzed with an HPLC. The limit of detection(LOD) of both indoxacarb and thiamethoxam was 0.01 mg $kg^{-1}$ and mean recoveries of indoxacarb and thiamethoxam were from 97.91 to 104.36% and from 97.07 to 105.49%, respectively. Half-lives of indoxacarb and thiamethoxam were 3.4 and 2.3 days at the recommended dose and 3.3 and 3.5 days at the doubled dose, respectively. The ratios of the EDI to ADI by intake the crop harvested 10 days after spraying were less than 4% of their ADIs.

Method Development for Determination of Multi-Mycotoxins in Chicken Liver and Kidney Tissues by LC-MS/MS (LC-MS/MS를 이용한 닭 간과 신장 중 곰팡이 독소 6종 동시분석법 개발)

  • Kim, Soohee;Kim, Kwang-Nam;Kim, Hyobi;Song, Jae-Young;Park, Sung-Won
    • Korean Journal of Poultry Science
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    • v.43 no.2
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    • pp.111-118
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    • 2016
  • Mycotoxins are secondary metabolites produced by molds, such as Aspergillus, Fusarium and Penicillium, that have adverse effects on animals and humans. Aflatoxin, ochratoxin, zearalenone, fumonisin and deoxynivalenol are the mycotoxins of greatest agro-economic importance and cause acute disease called mycotoxicoses. Mycotoxicosis in poultry birds results in decreased meat/egg production, immunosuppressant, and hepatotoxicosis. Some of toxins or their metabolites may be retained in animal or human tissues and induce health problems. This study was designed to develop a sensitive liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the simultaneous detection and quantification of mycotoxins, such as aflatoxin $B_1$, aflatoxin $M_1$, ochratoxin A, zearalenone, fumonisin B and deoxynivalenol, in chicken liver and kidney tissues. The mycotoxins were extracted and purified using modified QUECHERS methods, separated by LC and detected by an electrospray ionisation interface (ESI) and tandem MS. Good precision and linearity were observed for most of six mycotoxins. The recovery test for each mycotoxin in liver and kidney tissues mostly indicated good average recovery rates between 80.94% and 98.10% and the coefficient of variation mostly under 13.78%, except for aflatoxin $M_1$ and fumonisin $B_1$. The limit of detection (LOD) for six mycotoxins was $7.6{\sim}145.79{\mu}g/kg$ in liver tissues and $6.07{\sim}197.20{\mu}g/kg$ in kidney tissues. The quantification limits (LOQ) for 6 mycotoxins were in the range $23.04{\sim}441.78{\mu}g/kg$ in liver tissues and $18.40{\sim}597.59{\mu}g/kg$ in kidney tissues, respectively. The developed multi-mycotoxin method in this study permits simultaneous, simple, and rapid determination of several co-existing mycotoxins in chicken liver and kidney tissues.

A Comparative Study about Industrial Structure Feature between TL Carriers and LTL Carriers (구역화물운송업과 노선화물운송업의 산업구조 특성 비교)

  • 민승기
    • Journal of Korean Society of Transportation
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    • v.19 no.1
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    • pp.101-114
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    • 2001
  • Transportation enterprises should maintain constant and qualitative operation. Thus, in short period, transportation enterprises don't change supply in accordance with demand. In the result, transportation enterprises don't reduce operation in spite of management deficit at will. In freight transportation type, less-than-truckload(LTL) has more relation with above transportation feature than truckload(TL) does. Because freight transportation supply of TL is more flexible than that of LTL in correspondence of freight transportation demand. Relating to above mention, it appears that shortage of road and freight terminal of LTL is larger than that of TL. Especially in road and freight terminal comparison, shortage of freight terminal is larger than that of road. Shortage of road is the largest in 1990, and improved after-ward. But shortage of freight terminal is serious lately. So freight terminal needs more expansion than road, and shows better investment condition than road. Freight terminal expansion brings road expansion in LTL, on the contrary, freight terminal expansion substitutes freight terminal for road in TL. In transportation revenue, freight terminal's contribution to LTL is larger than that to TL. However, when we adjust quasi-fixed factor - road and freight terminal - to optimal level in the long run, in TL, diseconomies of scale becomes large, but in LTL, economies of scale becomes large. Consequently, it is necessary for TL to make counterplans to activate management of small size enterprises and owner drivers. And LTL should make use of economies of scale by solving the problem, such as nonprofit route, excess of rental freight handling of office, insufficiency of freight terminal, shortage of driver, and unpreparedness of freight insurance.

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Occurrence of Mycotoxins in Korean Grains and Their Simultaneous Analysis (한국산 곡류에서의 곰팡이독소 오염현황 및 동시분석)

  • Kim, Dong-Ho;Jang, Han-Sub;Choi, Gyu-Il;Kim, Hyun-Jung;Kim, Ho-Jin;Kim, Hyo-Lin;Cho, Hyun-Jung;Lee, Chan
    • Korean Journal of Food Science and Technology
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    • v.45 no.1
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    • pp.111-119
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    • 2013
  • Eleven mycotoxins, including aflatoxins, ochratoxin A, fumonisins, zearalenone, T-2 toxin, deoxynivalenol, and HT-2 toxin, were analyzed simultaneously in rice, barley, and maize produced in 2011 by liquid chromatography coupled with triple quadrupole mass spectrometry (LC/MS/MS). Limits of detection (LOD) are 0.2 ${\mu}g/kg$ for aflatoxin $B_1$, and $G_1$, 0.3 ${\mu}g/kg$ for aflatoxins $B_2$, and $G_2$, 0.1 ${\mu}g/kg$ for ochratoxin, fumonisins, zearalenone, and T-2 toxin and 3.0 ${\mu}g/kg$ for deoxynivalenol and HT-2 toxin. Limits of quantification (LOQ) were 0.6 ${\mu}g/kg$ for aflatoxins $B_1$, and $G_1$, 0.9 ${\mu}g/kg$ for aflatoxins $B_2$, and $G_2$, 0.3 ${\mu}g/kg$ for ochratoxin, fumonisins, zearalenone, and T-2 toxin and 10.0 ${\mu}g/kg$ for deoxynivalenol and HT-2 toxin. Recoveries for 11 mycotoxins ranged from 70.45 to 111.11%. Fumonisins, deoxynivalenol, and zaeralenone were detected from 0.9 to 334.0 ${\mu}g/kg$ in the polished rice, barley and raw corn cultivated in Korea. Other mycotoxins were not detected. Deoxynivalenol contamination was mainly found in barley (24 out of 43 samples) and the average value in positive samples was 113.30 ${\mu}g/kg$.

The Naturally Occurring Levels of Nitrate and Nitrite in Livestock Products (축산물 중 천연유래 질산염 및 아질산염 함유량 조사)

  • Choi, Jae-Chun;Park, So-Ra;Lim, Ho-Soo;Ko, Kyung-Yuk;Kim, Meehye
    • Journal of Food Hygiene and Safety
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    • v.30 no.3
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    • pp.265-271
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    • 2015
  • This study was done in order to investigate the naturally occurring levels of nitrate and nitrite in livestock products. Total samples of 458 consisting of meats (n = 223), processed meat products (n = 51), raw milks (n = 30), processed milk products (n = 142), eggs (n = 5) and processed egg products (n = 7) were analyzed for contents of nitrate and nitrite by ion chromatography (IC). That methods showed good results in terms of linearity, limit of detection (LOD), limit of quantitation (LOQ), recovery, reproducibility and uncertainty. Nitrate and nitrite were detected in 167 and 40 samples, respectively. The nitrate levels (mg/kg) were not detected (ND)~40.23 for modified milks, ND~37.97 for sauce meats, ND~32.40 for process cheeses, ND~31.50 for processed egg products, ND~27.73 for dry milks, ND~24.76 for sausages, ND~22.45 for bacons, ND~21.55 for natural cheeses, ND~20.82 for hams and fermented milks, ND~13.57 for eggs, ND~12.77 for butters, ND~9.31 for milks and ND~3.88 for meats while the nitrite levels (mg/kg) were ND~17.35 for processed egg products and ND~1.92 for meats. In conclusion, the result of this study of nitrate and nitrite in livestock products could be used as one of scientific base datum to determine whether they are naturally occurring or not, including ingredients and their percentage, manufacturing processes, other papers relating to naturally occurring levels of them, and so on.

Determination of Polycyclic Aromatic Hydrocarbons in Smoked Food Products (훈연식품 중 polycyclic aromatic hydrocarbons 함량 분석)

  • Seo, Ilwon;Nam, Hejung;Lee, Songyoung;Lee, Kyueun;Shin, Han-Seung
    • Food Engineering Progress
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    • v.13 no.3
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    • pp.195-202
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    • 2009
  • This study was accomplished that analysis of seven polycyclic aromatic hydrocarbons (PAHs) in smoked or nonsmoked processing foods by high performance liquid chromatography (HPLC) with fluorescence detection. The calibration line was constructed with injected different levels of standard concentration. Limit of detection (LOD) and limit of quantification(LOQ) showed higher linearity ($r^{2}$=0.998) reasonably, and recovery exhibited 0.033-0.666 $\mu$g/kg, 0.108-2.217 $\mu$g/kg and 69.31-90.14%, respectively. As a result, the samples using smoked tuna as smoked materials contained seven PAHs with different range from 0.256 to 0.486 $\mu$g/kg. The benzo[a]pyrene, indicator of PAHs, was detected to below the LOQ in two samples. Concentrations of benzo[a]pyrene in three samples were below the 2 $\mu$g/kg which is the limit of regulation. Smoked tuna sauces were detected from 0.321 to 0.552 $\mu$g/kg and not detected in drying powders. PAHs of smoked meat products were ranged from 0.720 to 2.027 $\mu$g/kg and are higher than concentration of tuna smoked samples. PAHs were very low in non-smoked foods including mustard, herb, and roasted meats.

Analytical Method for Sodium Polyacrylate in Processed Food Products by Using Size-exclusion Chromatography (Size-exclusion Chromatography를 활용한 가공식품 중 폴리아크릴산나트륨 분석법 확립)

  • Jeong, Eun-Jeong;Choi, Yoo-Jeong;Lee, Gunyoung;Yun, Sang Soon;Lim, Ho Soo;Kim, MeeKyung;Kim, Yong-Suk
    • Journal of Food Hygiene and Safety
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    • v.33 no.6
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    • pp.466-473
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    • 2018
  • An analytical method of sodium polyacrylate in processed food products was developed and monitored by using size-exclusion chromatography. GF-7M HQ column and UV/VIS detector were selected based on peak shape and linearity. Flow rate, column oven temperature, and mobile phase were selected as 0.6 mL/min, $45^{\circ}C$, and 50 mM sodium phosphate buffer of pH 9.0, respectively. Samples for analysis of sodium polyacrylate were extracted with 50 mM sodium phosphate buffer of pH 7.0 for 3 hr at $20^{\circ}C$ and 150 rpm. Analytical method validation revealed proper selectivity and calibration curve was selected in the range of 50-500 mg/L, and correlation coefficient of calibration curve was more than 0.9985. Limit of detection of sodium polyacrylate was 10.95 mg/kg and limit of quantification was 33.19 mg/kg. Accuracy and coefficient of variation for sodium polyacrylate analysis was 99.6-127.6%, 3.0-8.3% for intra-day and 94.3-121.9%, 1.3-2.6% for inter-day, respectively. Sodium polyacrylate was detected in 40 samples among monitored 125 processed food products. Detected contents were less than 0.2%, limited by the Food Additives Code. Results suggest the established size-exclusion chromatography method could be used to analyze sodium polyacrylate in processed food products.

Validation of Stem-loop RT-qPCR Method on the Pharmacokinetic Analysis of siRNA Therapeutics (Stem-loop RT-qPCR 분석법을 이용한 siRNA 치료제의 생체시료 분석법 검증 및 약물 동태학적 분석)

  • Kim, Hye Jeong;Kim, Taek Min;Kim, Hong Joong;Jung, Hun Soon;Lee, Seung Ho
    • Journal of Life Science
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    • v.29 no.6
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    • pp.653-661
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    • 2019
  • The first small interfering RNA (siRNA) therapeutics have recently been approved by the Food and Drug Administration in the U.S., and the demand for a new RNA therapeutics bioanalysis method-which is essential for pharmacokinetics, including the absorption, distribution, metabolism, and excretion of siRNA therapeutics-is rapidly increasing. The stem-loop real-time qPCR (RT-qPCR) assay is a useful molecular technique for the identification and quantification of small RNA (e.g., micro RNA and siRNA) and can be applied for the bioanalysis of siRNA therapeutics. When the anti-HPV E6/E7 siRNA therapeutic was used in preclinical trials, the established stem-loop RT-qPCR assay was validated. The limit of detection was sensitive up to 10 fM and the lower limit of quantification up to 100 fM. In fact, the reliability of the established test method was further validated in three intra assays. Here, the correlation coefficient of $R^2$>0.99, the slope of -3.10 ~ -3.40, and the recovery rate within ${\pm}20%$ of the siRNA standard curve confirm its excellent robustness. Finally, the circulation profiles of siRNAs were demonstrated in rat serum, and the pharmacokinetic properties of the anti-HPV E6/E7 siRNA therapeutic were characterized using a stem-loop RT-qPCR assay. Therefore, the stemloop RT-qPCR assay enables accurate, precise, and sensitive siRNA duplex quantification and is suitable for the quantification of small RNA therapeutics using small volumes of biological samples.