• Title/Summary/Keyword: Relative quantification

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Optimization of solid-phase extraction for the liquid chromatography-tandem mass spectrometry analysis of basic drugs in equine urine (액체크로마토그래피-텐덤질량분석법을 위한 경주마 소변 중 염기성 약물의 고체상 추출법 최적화)

  • Shin, Hyun Du;Yang, Ji Suk;Jung, Mihye;Kim, Hyung-Seung;Youm, Jeong-Rok;Hu, Man Bae;Kim, Sung Jean;Han, Sang Beom
    • Analytical Science and Technology
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    • v.21 no.5
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    • pp.412-423
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    • 2008
  • A procedure based on solid-phase extraction (SPE) followed by liquid chromatography-tandem mass spectrometry has been developed for the simultaneous analysis of 55 basic drugs in equine urine. The test scope covers diversified classes of drugs including some ${\beta}$-blockers, ${\beta}$-agonists, antihypotensives, CNS stimulants, sedatives, tranquilizers, antidepressants, antihypertensives and so on. LC-MS/MS separation and quantification was carried out in positive electrospray ionization and multiple reaction monitoring (MRM) mode. Four different brands of mixed mode cation exchange SPE sorbents; UCT XTRACT$^{(R)}$ XRDAH, Supelco DSC-MCAX$^{(R)}$, Varian Bond Elut Certify$^{(R)}$ and Waters Oasis$^{(R)}$ MCX were compared. The UCT XTRACT$^{(R)}$ XRDAH sorbent provided the best results in the preconcentration of samples, yielding relative recoveries higher than 80% except for terbutaline (41.3%), salbutamol (71.5%), heptaminol (70.7%), phenylpropanolamine (66.3%). Detection limits of the target drugs provided by the proposed analytical procedure were between 0.2~8.3 ng/mL.

Antioxidant activities and Validation of Analytical Method of Marker compounds in strawberry fruits from various cultivars (딸기 품종별 추출물의 항산화활성 및 지표성분 밸리데이션)

  • Yong, Ye Seul;Lee, Songmi;Byun, Na-Young;Sun, Sangouk;Kim, Min-Jung;Jang, Seo Woo;Jang, Won Suk;Lee, Sun Yi;Yim, Soon-Ho
    • Korean Journal of Food Science and Technology
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    • v.51 no.6
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    • pp.517-523
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    • 2019
  • In this study, we investigated antioxidant capacity of 20 strawberry extract using the DPPH and ABTS assay and HPLC-DAD validation method. The total polyphenolic and flavonoids contents of 20 strawberry extracts were 22.77-107.61 mg TAE/100 g FW and 17.58-44.12 mg QE/100 g FW. The Aiberry and Elie star showed the highest total polyphenol and flavonoid contents, respectively. The DPPH radical scavenging activity of what was 1540.6-1124.0 μmol TEAC/100 g FW and Derunoka showed the highest activity. The ABTS radical scavenging activity was 6352.3-4592.3 μmol TEAC/100 g FW and FA23 showed the highest activity. The HPLC-DAD method for the quantitation of ellagic acid results showed high linearity in various concentration ranges, and the limit of detection was 2.35 μg/mL. The limit of quantification was 7.12 μg/mL. Relative standard deviation values from intra-and inter-day precision were less than 5.31%. Recovery rate at 10, 50, and 100 μg/mL, respectively, were 100.0-101.0% with relative standard deviation (RSD) values less than 5.30%. These results provide viable information for the validation of antioxidant capacity in strawberry fruits.

Mineralogical Characteristics of the Lower Choseon Supergroup in the Weondong Area (원동지역 하부 조선누층군의 광물학적 특성)

  • Kim, Ha;Sim, Ho;Won, Moosoo;Kim, Myeong-Ji;Lee, Ju-Ho;Song, Yun-Goo
    • Economic and Environmental Geology
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    • v.49 no.5
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    • pp.349-360
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    • 2016
  • This study determined mineralogical characteristics and discussed the meaning of mineralogical changes of the lower Choseon Supergrouop in the Weondong area based on the field geological investigation and the drilling core description using X-ray diffraction (XRD) mineral quantification and Scanning Electron Microscopy (SEM) observation. 100 samples with depth were collected from the core (250 m long) at a site in the study area. Especially, to investigate the changes from the upper Daegi Formation to the lower Hwajeol Formation, the samples were collected closely with the interval of about 0.3 m at this section. All samples were made into power using mortar for XRD. Mineral quantitative analysis was executed using Relative Intensity Ratio (RIR) method with corundum as an internal standard phase. Calcite, $2M_1$ illite and quartz are main constituents in most of samples. Dolomite and siderite are significantly observed in the Sesong Formation. As the results of quantitative analysis for the major minerals, the upper Daegi Formation is dominated by calcite with over 80%. The Sesong Formation includes high percentage of dolomite and siderite with the intercalation of thin layers containing high calcite and $2M_1$ illite contents. Hwajeol Formation is characterized by the alternation between thin layers of $2M_1$ illite and quartz-dominated layer (IQDL) and calcite-dominated layer (CDL). IQDL is more frequent in the lower part, whereas CDL is more common in the upper part. The boundary between Daegi Formation and the Sesong Formation is distinct, whereas the boundary between the Sesong Formation and the Hwajeol Formation tends to be changed gradually in mineralogy. The result of SEM observation shows that quartz and $2M_1$ illite are detrital, and a significant amount of calcite also shows detrital form with some recrystallized one, indicating that the repeated influx of terrestrial materials had changed the mineralogy of the shallow sea depositional environment in the early Paleozoic era.

Development and Validation of an Analytical Method for Determination of Fungicide Tridemorph in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 tridemorph의 시험법 개발 및 검증)

  • Pak, Won-Min;Do, Jung-Ah;Lim, Seung-Hee;Park, Shin-Min;Yoon, Ji-Hye;Lee, Dong-seouk;Chang, Moon-Ik
    • Journal of Food Hygiene and Safety
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    • v.32 no.4
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    • pp.290-297
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    • 2017
  • The purpose of this study was developed for the determination of tridemorph in agricultural commodities samples. Tridemorph residues in samples were extracted with acetonitrile, partitioned with saline water, and then purified using and aminopropyl ($NH_2$) SPE catridge. The purified samples were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005~2.5 ng) into a blank extract with $r^2$ > 0.999. The limits of detection and quantification were 0.001 and 0.005 mg/kg, respectively. The average recovery ranged between 75.9% and 103.7% at different concentration levels (LOQ, 10 LOQ, 50 LOQ, n = 5) with relative standard deviations (RSDs) less than 9.0%. An interlaboratory study was conducted to validate the method by Korea Advanced Food Research Institute. The average recovery ranged between 87.0% and 109.2% at different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$, n = 5) with relative standard deviations (RSDs) less than 8.0%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003) and Food Safety Evaluation Department guidelines (2016). The results prove that the developed analytical methods is accurate, effective and sensitive for tridemorph determination.

Development of Analytical Method for Kasugamycin in Agricultural Products using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Kasugamycin 시험법 개발)

  • Lee, Han Sol;Do, Jung-Ah;Park, Ji-Su;Cho, Sung Min;Shin, Hye-Sun;Jang, Dong Eun;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.3
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    • pp.235-241
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    • 2019
  • An analytical method was developed for the determination of an antibiotic fungicide, kasugamycin, in agricultural products (hulled rice, potato, soybean, mandarin and green pepper) using liquid chromatographytandem mass spectrometry (LC-MS/MS). Samples were extracted with methanol adjusted to pH 13 using 1 N sodium hydroxide, and purified with a HLB (hydrophilic lipophilic balance) cartridge. Linearity of a matrix-matched calibration curve using seven concentration levels, from 0.001 to 0.1 mg/kg, was excellent with a correlation coefficient ($R^2$) of more than 0.9998. The limits of detection (LOD) and quantification (LOQ) of instrument were 0.0005 and $0.001{\mu}g/mL$, respectively, and the LOQ of analytical method calculated as 0.01 mg/kg. The average recoveries at three spiking levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) were in the range of 71.2~95.4% with relative standard deviation of less than 12.1%. The developed method was simple and all optimized results was satisfied with the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. The present study could be served as a reference for the establishment of maximum residue limits (MRL) of kasugamycin and be used as basic data for safety management relative to kasugamycin residues in imported and domestic agricultural products.

Development and Validation of an Official Analytical Method for Determination of Ipfencarbazone in Agricultural Products using GC-ECD (GC-ECD를 이용한 농산물 중 Ipfencarbazone의 신규분석법 개발 및 검증)

  • Jang, Jin;Kim, Heejung;Lee, Eun-Hyang;Ko, Ah-Young;Ju, Yunji;Kim, Sooyeon;Chang, Moon-Ik;Rhee, Gyu-Seek
    • The Korean Journal of Pesticide Science
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    • v.19 no.3
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    • pp.210-217
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    • 2015
  • Ipfencarbazone is a herbicide of the tetrazolinone class, and is believed to be an inhibitor of very long chain fatty acids (VLCFAs), which control cell division in weeds. The objective of this study was to develop and validate an official analytical method for ipfencarbazone determination in agricultural products. The ipfencarbazone residues in agricultural products were extracted with acetone, partitioned with n-hexane, and then purified through silica SPE cartridge. Finally, the analyte was quantified by gas chromatograph-electron capture detector (GC-ECD) and confirmed with gas chromatograph/mass spectrometer(GC/MS). The linear range of ipfencarbazone was 0.01 to 1.0 mg/L with the coefficient of determination ($r^2$) of 0.9999. The limit of detection (LOD) and quantification (LOQ) was 0.003 and 0.01 mg/kg, respectively. In addition, average recoveries of ipfencarbazone ranged from 80.6% to 112.3% at the different concentration levels LOQ, 10LOQ and 50LOQ, while the relative standard deviation was 2.2-8.6%. All values were consistent with the criteria ranges requested in the CODEX guidelines. Furthermore, and inter-laboratory study was conducted to validate the method. This proposed method for determination of ipfencarbazone residues in agricultural products can be used as an official analytical method.

Gas Chromatographic Method for Multiresidue Analysis of Unregistered Pesticides in Imported Agricultural Commodities (가스 크로마토그래피를 이용한 수입농산물 중 국내 미등록 농약의 다성분 동시분석법 적용)

  • Lee, Ji-Won;Kang, Jeong-Kyun;Kwon, Hyeyoung;Ro, Jin-Ho;Jin, Yong-Duk;Lee, Je Bong;Hong, Su-Myeoung;Kim, Teak-Kyum;Cho, Nam-Jun
    • The Korean Journal of Pesticide Science
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    • v.19 no.3
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    • pp.161-173
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    • 2015
  • The multiresidue method 4.1.2.2 in Korea Food Code was extended for the analysis of 24 unregistered pesticide residues. The method includes acetonitrile extraction, liquid-liquid partition, Florisil SPE clean-up and GC analysis. The limits of quantification (LOQ) range of the method was 0.02~0.05 mg/kg for orange, brown rice and banana. The linearity for targeted pesticides were $R^2$ > 0.99 at the level ranged from 0.05 to 5 mg/L. Recovery test was performed at two concentration levels of LOQ and 4~10 times of LOQ. Recoveries and relative standard deviations (RSDs) of target pesticides were acceptable, showing 70~120% range and less than 20%, respectively, except for ethiprole, picloram and sulcotrion. This method is effectively applicable to routine analysis of target pesticides in orange, brown rice and banana.

Optimization of Analytical Methods for Ochratoxin A and Zearalenone by UHPLC in Rice Straw Silage and Winter Forage Crops (UHPLC를 이용한 볏짚 사일리지와 동계사료작물의 오크라톡신과 제랄레논 분석법 최적화)

  • Ham, Hyeonheui;Mun, Hye Yeon;Lee, Kyung Ah;Lee, Soohyung;Hong, Sung Kee;Lee, Theresa;Ryu, Jae-Gee
    • Journal of The Korean Society of Grassland and Forage Science
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    • v.36 no.4
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    • pp.333-339
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    • 2016
  • The objective of this study was to optimize analytical methods for ochratoxin A (OTA) and zearalenone (ZEA) in rice straw silage and winter forage crops using ultra-high performance liquid chromatography (UHPLC). Samples free of mycotoxins were spiked with $50{\mu}g/kg$, $250{\mu}g/kg$, or $500{\mu}g/kg$ of OTA and $300{\mu}g/kg$, $1500{\mu}g/kg$, or $3000{\mu}g/kg$ of ZEA. OTA and ZEA were extracted by acetonitrile and cleaned-up using an immunoaffinity column. They were then subjected to analysis with UHPLC equipped with a fluorescence detector. The correlation coefficients of calibration curves showed high linearity ($R^2{\geq_-}0.9999$ for OTA and $R^2{\geq_-}0.9995$ for ZEA). The limit of detection and quantification were $0.1{\mu}g/kg$ and $0.3{\mu}g/kg$, respectively, for OTA and $5{\mu}g/kg$ and $16.7{\mu}g/kg$, respectively, for ZEA. The recovery and relative standard deviation (RSD) of OTA were as follows: rice straw = 84.23~95.33%, 2.59~4.77%; Italian ryegrass = 79.02~95%, 0.86~5.83%; barley = 74.93~97%, 0.85~9.19%; rye = 77.99~96.67%, 0.33~6.26%. The recovery and RSD of ZEA were: rice straw = 109.6~114.22%, 0.67~7.15%; Italian ryegrass = 98.01~109.44%, 1.65~4.81%; barley = 98~113.53%, 0.25~5.85%; rye = 90.44~108.56%, 2.5~4.66%. They both satisfied the standards of European Commission criteria (EC 401-2006) for quantitative analysis. These results showed that the optimized methods could be used for mycotoxin analysis of forages.

Effects of Attenuation and Scatter Corrections in Cat Brain PET Images Using microPET R4 Scanner (MicroPET R4 스캐너에서 획득한 고양이 뇌 PET 영상의 감쇠 및 산란보정 효과)

  • Kim, Jin-Su;Lee, Jae-Sung;Lee, Jong-Jin;Lee, Byeong-Il;Park, Min-Hyun;Lee, Hyo-Jeong;Oh, Seung-Ha;Kim, Kyeong-Min;Cheon, Gi-Jeong;Lim, Sang-Moo;Chung, June-Key;Lee, Myung-Chul;Lee, Dong-Soo
    • Nuclear Medicine and Molecular Imaging
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    • v.40 no.1
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    • pp.40-47
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    • 2006
  • Purpose: The aim of this study was to examine the effects of attenuation correction (AC) and scatter correction (SC) on the quantification of PET count rates. Materials and Methods: To assess the effects of AC and SC $^{18}F$-FDG PET images of phantom and cat brain were acquired using microPET R4 scanner. Thirty-minute transmission images using $^{68}Ge$ source and emission images after injection of FDG were acquired. PET images were reconstructed using 2D OSEM. AC and SC were applied. Regional count rates were measured using ROIs drawn on cerebral cortex including frontal, parietal, and latral temporal lobes and deep gray matter including head of caudate nucleus, putamen and thalamus for pre- and post-AC and SC images. The count rates were then normalized with the injected dose per body weight. To assess the effects of AC, count ratio of "deep gray matter/cerebral cortex" was calculated. To assess the effects of SC, ROIs were also drawn on the gray matter (GM) and white matter (WM), and contrast between them ((GM-WM)/GM was measured. Results: After the AC, count ratio of "deep gray matter/cerebral cortex" was increased by $17{\pm}7%$. After the SC, contrast was also increased by $12{\pm}3%$. Conclusion: Relative count of deep gray matter and contrast between gray and white matters were increased after AC and SC, suggesting that the AC would be critical for the quantitative analysis of cat brain PET data.

Development of an Official Analytical Method for Determination of Aclonifen in Agricultural Products Using GC-ECD (GC-ECD를 이용한 농산물 중 제초제 aclonifen의 공정분석법 확립)

  • Ko, Ah-Young;Kim, Hee-Jung;Jang, Jin;Lee, Eun-Hyang;Joo, Yoon-Ji;Kwon, Chan-Hyeok;Son, Young-Wook;Chang, Moon-Ik;Rhee, Gyu-Seek
    • Korean Journal of Environmental Agriculture
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    • v.33 no.4
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    • pp.388-394
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    • 2014
  • BACKGROUND: Aclonifen is used as a systemic and selective herbicide to control a wide spectrum broad-leaf weeds by inhibition carotenoid biosynthesis, and then its MRLs(Maximum Residue Limits) will be determined in onion and garlic. In this study, a new official method was developed for aclonifen determination in agricultural products to routinely inspect the violation of MRL as well as to evaluate the terminal residue level. METHODS AND RESULTS: Aclonifen was extracted from crop samples with acetone and the extract was partitioned with dichloromethane and then purified by silica solid phase extraction(SPE) cartridge. The purified samples were detected GC using an ECD detector. Limits of detection(LOD) was 0.001 mg/kg and quantification(LOQ) was 0.005 mg/kg, respectively. For validation purposes, recovery studies were carried out at three different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$, n=5). The recoveries were ranged from 74.3 to 95.0% with relative standard deviations(RSDs) of less than 8%. All values were consistent with the criteria ranges requested in the Codex guidelines(CAC/GL 40). CONCLUSION: The proposed analytical method was accurate, effective and sensitive for aclonifen determination and it will be used to as an official method in Korea.