• Title/Summary/Keyword: Calibration method

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Residual evaluation of ethyl formate in soil and crops after fumigation in green house (에틸포메이트의 하우스 농작물 훈증처리 후 토양 및 작물 중 잔류양상)

  • Hwang-Ju Jeon;Kyeongnam Kim;Chaeeun Kim;Yerin Cho;Tae-Hyung Kwon;Byung-Ho Lee;Sung-Eun Lee
    • Korean Journal of Environmental Biology
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    • v.40 no.3
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    • pp.316-324
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    • 2022
  • Ethyl formate (EF) is a potent fumigant replacing methyl bromide. The use of EF is limited to a quarantine process. Appling EF to agricultural field as a safe insecticide in greenhouse give us valuable benefits including less residual concern. In this regard, residual pattern after EF fumigation in greenhouse should be undertaken. In the previous study, we have established agricultural control concentration of EF to control pests in a greenhouse. EF was fumigated at 5 g m-3 level for 2 h. The concentration of EF inside a greenhouse was analyzed to be 4.1-4.3 g m-3 at 30 min after fumigation. To prepare an analytical method for residues in cucumber crops and soil in the greenhouse, the limit of detection(LOD) of the method was 100ng g-1 and the limit of quantitation(LOQ) of this method was 300 ng g-1. R2 values of calibration curves for crops and soil were 0.991-0.997. In samples collected immediately after ventilation, EF concentration was determined to be below LOQ level. In addition, EF level was below LOQ in samples collected at 3 h after ventilation except that leaf samples of melon during the flowering period showed a level of 1,068.9 ng g-1. Taken together, these results indicate that EF used in quarantine can be applied to agricultural fields without residual issue as an effective fumigant for insect pest control.

Application and Analysis of Ocean Remote-Sensing Reflectance Quality Assurance Algorithm for GOCI-II (천리안해양위성 2호(GOCI-II) 원격반사도 품질 검증 시스템 적용 및 결과)

  • Sujung Bae;Eunkyung Lee;Jianwei Wei;Kyeong-sang Lee;Minsang Kim;Jong-kuk Choi;Jae Hyun Ahn
    • Korean Journal of Remote Sensing
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    • v.39 no.6_2
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    • pp.1565-1576
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    • 2023
  • An atmospheric correction algorithm based on the radiative transfer model is required to obtain remote-sensing reflectance (Rrs) from the Geostationary Ocean Color Imager-II (GOCI-II) observed at the top-of-atmosphere. This Rrs derived from the atmospheric correction is utilized to estimate various marine environmental parameters such as chlorophyll-a concentration, total suspended materials concentration, and absorption of dissolved organic matter. Therefore, an atmospheric correction is a fundamental algorithm as it significantly impacts the reliability of all other color products. However, in clear waters, for example, atmospheric path radiance exceeds more than ten times higher than the water-leaving radiance in the blue wavelengths. This implies atmospheric correction is a highly error-sensitive process with a 1% error in estimating atmospheric radiance in the atmospheric correction process can cause more than 10% errors. Therefore, the quality assessment of Rrs after the atmospheric correction is essential for ensuring reliable ocean environment analysis using ocean color satellite data. In this study, a Quality Assurance (QA) algorithm based on in-situ Rrs data, which has been archived into a database using Sea-viewing Wide Field-of-view Sensor (SeaWiFS) Bio-optical Archive and Storage System (SeaBASS), was applied and modified to consider the different spectral characteristics of GOCI-II. This method is officially employed in the National Oceanic and Atmospheric Administration (NOAA)'s ocean color satellite data processing system. It provides quality analysis scores for Rrs ranging from 0 to 1 and classifies the water types into 23 categories. When the QA algorithm is applied to the initial phase of GOCI-II data with less calibration, it shows the highest frequency at a relatively low score of 0.625. However, when the algorithm is applied to the improved GOCI-II atmospheric correction results with updated calibrations, it shows the highest frequency at a higher score of 0.875 compared to the previous results. The water types analysis using the QA algorithm indicated that parts of the East Sea, South Sea, and the Northwest Pacific Ocean are primarily characterized as relatively clear case-I waters, while the coastal areas of the Yellow Sea and the East China Sea are mainly classified as highly turbid case-II waters. We expect that the QA algorithm will support GOCI-II users in terms of not only statistically identifying Rrs resulted with significant errors but also more reliable calibration with quality assured data. The algorithm will be included in the level-2 flag data provided with GOCI-II atmospheric correction.

Development and Validation of the Analytical Method for Oxytetracycline in Agricultural Products using QuEChERS and LC-MS/MS (QuEChERS법 및 LC-MS/MS를 이용한 농산물 중 Oxytetracycline의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Cho, Myong-Shik;Jung, ong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.3
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    • pp.227-234
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    • 2019
  • An analytical method was developed for the determination of oxytetracycline in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). After the samples were extracted with methanol, the extracts were adjusted to pH 4 by formic acid and sodium chloride was added to remove water. Dispersive solid phase extraction (d-SPE) cleanup was carried out using $MgSO_4$ (anhydrous magnesium sulfate), PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed with LC-MS/MS using ESI (electrospray ionization) in positive ion MRM (multiple reaction monitoring) mode. The matrix-matched calibration curves were constructed using six levels ($0.001{\sim}0.25{\mu}g/mL$) and coefficient of determination ($r^2$) was above 0.99. Recovery results at three concentrations (LOQ, $10{\times}LOQ$, and $50{\times}LOQ$, n=5) were from 80.0 to 108.2% with relative standard deviations (RSDs) less than of 11.4%. For inter-laboratory validation, the average recovery was in the range of 83.5~103.2% and the coefficient of variation (CV) was below 14.1%. All results satisfied the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for oxytetracycline determination in agricultural commodities. This study could be useful for safety management of oxytetracycline residues in agricultural products.

A study of relationship between stomach cancer and selenoproteins in Korean human blood serum (한국인 혈청에서의 셀레노 단백질과 위암과의 상관관계 연구)

  • Park, Myungsun;Pak, Yong-Nam
    • Analytical Science and Technology
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    • v.28 no.6
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    • pp.417-424
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    • 2015
  • In this study, the relationship between selenoprotein concentrations in blood and stomach cancer have been searched for Korean. The concentration of each selenoprotein in blood serum was analyzed and the correlation between the concentration and stomach cancer was studied to find a potential for using Selenium as a biomarker. In concentration determination, a simple calibration curve method was used with the monitoring of m/z 78 without the use of solid phase extraction. This is a lot more simple than the method using SPE with post column isotope dilution. The result obtained from the analysis of CRM BCR-637, 72.20±3.35 ng·g−1, showed similar value of reference value (81±7 ng·g−1). The total concentration of Se for the controlled group, cardiovascular patients group, was 105.70±21.20 ng·g−1. This value was the same as normal healthy person reported earlier. Each selenoprotein concentration of GPx, SelP and SeAlb was 26.12±7.84, 65.15±14.50, 14.43±6.99 ng·g−1, respectively. The distribution of each selenoprotein was 24.7%, 61.6%, and 13.7%, which was similar to the normal person. The result of stomach cancer patients, the total concentration of Se was 76.11±28.12 ng·g−1 and each concentration of GPx, SelP and SeAlb was 15.41±9.01, 50.83±17.91, and 9.87±5.21 ng·g−1, respectively. The total and each selenoprotein concentration level showed significant decrease for the stomach cancer patients. The level of decrease was 41.0% for GPx, 22.0% for SelP, and 31.6% for SeAlb. However, the distribution of each selenoprotein was not much different. Either total Selenium or each selenoprotein could be used as a possible index for the diagnosis of cancer. However, in age group study, it is shown that young age group (30's-40's) did not show much difference.

Simultaneous Determination of Eight Sugar Alcohols in Foodstuffs by High Performance Liquid Chromatography (HPLC를 이용한 식품 중 당알코올 8종 동시분석)

  • Lim, Ho-Soo;Park, Sung-Kwan;Kwak, In-Shin;Kim, Hyung-Il;Sung, Jun-Hyun;Choi, Jung-Yoon;Kim, So-Hee
    • Journal of Food Hygiene and Safety
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    • v.26 no.1
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    • pp.16-24
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    • 2011
  • A method was established for the simultaneous determination of sugar alcohols, erythritol, xylitol, sorbitol, inositol, mannitol, maltitiol, lactitol and isomalt by High Performance Liquid Chromatography (HPLC). The sugar alcohols were converted into strong ultraviolet (UV)-absorbing derivatives with p-nitrobenzoyl chloride (PNBC). HPLC was performed on Imtakt Unison US-$C_18$ column, using acetonitrile: water (77:23) as a mobile phase and UV detection (260 nm). The calibration curves for all sugar alcohols tested were linear in the 10~200 mg/L range. The average recoveries of the sugar alcohols from three confectioneries spiked at 100 ppm of eight sugar alcohol standards ranged from 81.2 to 123.1% with relative standard deviations ranging fromo 0.2 to 4.9%. The limits of detection (LODs) were $0.5{\sim}8\;{\mu}g/L$ and the limits of quantification (LOQs) were $2{\sim}17\;{\mu}g/L$. Reproducibility of 8 sugar alcohols was 0.28~1.97 %RSD. The results of the analysis of confectioneries showed that 89 samples of 130 were detected and the sugar alcohols content of samples investigated varied between 0.4 and 693.7 g/kg. A method for the simultaneous determination of eight sugar alcohols will be used as basic data for control of sugar alcohols in confectioneries, and quality control in food manufacturing.

Determination of finasteride in human serum by LC-MS/MS (LC-MS/MS를 이용한 혈청 중 finasteride 분석)

  • Nam, Hye-Seon;Nam, Kyong-Hee;Jung, Su-Hee;Lee, Jang-Woo;Kang, Jin-Yeong;Hong, Soon-Keun;Kim, Tae-Sung;Kang, Tae-Seok;Yoon, Hae-Jung;Lee, Kwang-Ho;Rhee, Gyu-Seek
    • Analytical Science and Technology
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    • v.24 no.5
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    • pp.345-351
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    • 2011
  • A liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) method was developed and validated for the determination of finasteride in human serum. Beclomethasone was used as internal standard (IS) and liquid-liquid extraction (LLE) using methyl tert-butyl ether (MTBE) was carried out to isolate analyte. The mass transitions monitored in multiple reaction monitoring (MRM) in positive ion mode were m/z 373.2${\rightarrow}$305.2 for finasteride and m/z 409.3${\rightarrow}$391.2 for IS. Retention times of finasteride and IS were 5.81 and 5.46 min, respectively. The limit of quantitation (LOQ) was 0.1 ng/mL and the calibration curve showed good linearity in the range of 0.1~20.0 ng/mL ($R^2$=0.9997). The intra-day assay precision and accuracy were in the range 6.3~10.6% and 97.3~103.6%, respectively, and the inter-day assay precision and accuracy were in the range 0.8~5.2% and 99.8~102.5%, respectively. The sample extract recovery of the method was 80~83%.

Determination of homogentisic acid in human plasma by GC-MS for diagnosis of alkaptonuria (GC-MS를 이용한 혈장 중 호모겐티식산의 분석;알캅톤뇨증의 진단)

  • Thapa, Maheshwor;Yu, Jundong;Lee, Wonjae;Islam, Fokhrul;Yoon, Hye-Ran
    • Analytical Science and Technology
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    • v.28 no.5
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    • pp.323-330
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    • 2015
  • Alkaptonuria, a rare inherited metabolic disease, is characterized by a lack of homogentisate dioxygenase and accumulation of homogentisic acid (HGA), leading to homogentisic aciduria, arthritis, and ochronosis. In this study, a rapid analytical method, without an expensive and tedious solid phase extraction step, was developed to quantify HGA in plasma using GC-MS. HGA-spiked pooled plasma samples were subjected to liquid-liquid extraction (LLE) with ethyl acetate, followed by trimethylsilyl derivatization (TMS) and GC-MS quantification using selected ion monitoring. The formation of TMS derivative of the 1 carboxylic and 2 hydroxyl functional groups was performed by reacting BSTFA (with 10% TMCS) for 5 min at 80 ℃. For selected ion monitoring, quantification and confirmation ions were determined based on specific ions (m/z 384, m/z 341 and m/z 252) of the TMS derivative of HGA. Calibration curves of pooled normal plasma specimens showed a linear relationship in the range of 1-100 ng/µL. The precision and accuracy were within a relative standard deviation (RSD) of 1 to 15% and a bias of -5 to 25%. Recoveries were obtained in the range of 99-125% and 95-115% for intra-day and inter-day assay, respectively, at 2, 20 and 80 ng/µL. The limit of detection (LOD) and limit of quantification (LOQ) were 0.4 ng/µL and 4 ng/µL, respectively. No homogentisic acid was excreted from normal Korean plasma samples. Collectively, the results from the present study suggest that this method could be useful for routine diagnosis and therapeutic monitoring of alkaptonuria patients with excellent sensitivity and rapidity.

Nasal Continuous Positive Airway Pressure Titration and Time to Reach Optima1 Pressure in Sleep Apnea Syndrome (수면 무호흡 증후군에서 지속적 양압 치료시의 최적압 및 그 도달기간)

  • Lee, Kwan-Ho;Lee, Hyun-Woo
    • Tuberculosis and Respiratory Diseases
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    • v.42 no.1
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    • pp.84-92
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    • 1995
  • Background: Nasal applied continuous positive airway pressure(CPAP) is a highly effective method of treatment for obstructive sleep apnea syndrome. More than a decade of accumulated experience with this treatment modality confirmed that it is unquestionably the medical treatment of choice for patients with obstructive sleep apnea syndrome. However it takes long time to reach optimal CPAP pressure. To save the time to reach optimal pressure, it is necessary to clarify the time to reach optimal pressure for treatment of obstructive sleep apnea syndrome. Method: CPAP pressure is titrated during an overnight study according to a standardized protocol. Just before the presleep bio-calibration procedures, the technician applies the nasal mask and switches on the clinical CPAP unit. Initial positive for pressure is typically 3.0 centimeters of water pressure. After sleep onset, the technician gradually increases the pressure until sleep-disordered breathing events disappear or become minimal. The pressure must maintain maximal airway patency during both NREM and REM sleep to be considered effective. Before recommending a final pressure setting, sleep recording and oximetry data are reviewed by an American Board of Sleep Medicine certified Sleep Specialist and a Registrered Polysomnographic Technologist. Results: We examined the time required to reach optimal pressure during routine CPAP titration in 127 consecutively evaluated individuals diagnosed with sleep-disordered breathing. Results indicate that 33% of patients required more than four hours to attain satisfactory titration. This indicates that a four-hour session is marginally enough time, at best, to determine a proper CPAP pressure setting. Moreover, 60 of 127 patients required further adjustment after optimal pressure was reached. These additional pressure trials were needed to confirm that higher pressures were not superior for eliminating sleep-disordered breathing events. Conclusions: The data presented underscore the logistical difficulty of titrating CPAP during split-night studies without modifying the titration procedure. Futhermore, the time needed to reach optimal pressure makes it improbable that proper CPAP titration can be performed during a 2-3 hour nap study.

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Vitamin C Quantification of Korean Sweet Potatoes by Cultivar and Cooking Method (국내산 고구마의 품종 및 조리방법별 비타민 C 함량)

  • Hwang, In Guk;Byun, Jae Yoon;Kim, Kyung Mi;Chung, Mi Nam;Yoo, Seon Mi
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.43 no.6
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    • pp.955-961
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    • 2014
  • This study was carried out to investigate the amounts of vitamin C in 22 sweet potato cultivars cultivated in Korea as well as evaluate the effects of cooking methods on vitamin C contents. Methods for determining vitamin C was validated by determining linearity, specificity, limit of detection (LOD), limit of quantification (LOQ), precision, and accuracy using HPLC. Results showed high linearity in the calibration curve with a coefficient of correlation ($R^2$) of 0.9999. The LOD and LOQ values for ascorbic acid (AA) were 0.03 and $0.10{\mu}g/mL$, respectively. The relative standard deviations (RSDs) for intra- and inter-day precision of AA were less than 5%. The recovery rates of AA and dehydroascorbic acid (DHA) were in the range from 98.21~98.64 and 98.28~100.68%, respectively. Depending on cultivar, contents of AA, DHA, and total ascorbic acid (TA) in sweet potatoes varied in the range from 37.76 (Sinyulmi)~89.25 (Juhwangmin), 23.37 (Sinjami)~63.94 (Sinyulmi), and 68.52 (Sinjami)~115.95 (Juhwangmin) mg/100 g, respectively, and their average levels were $56.98{\pm}12.53$, $36.46{\pm}9.03$, and $93.44{\pm}12.00mg/100g$, respectively. The average TA levels were also dependent on flesh color, whish was significantly higher in general sweet potato and orange sweet potato than in purple sweet potato. Steaming, baking, and frying processes significantly reduced AA (10.61~58.41%), DHA (2.57~52.81%), and TA (14.54~49.92%) contents in sweet potatoes. The highest reduction of AA, DHA, and TA contents was observed after baking, followed by steaming and frying. We expect that the basic information provided by this study will be useful to plant breeders and food scientists.

Determination of aromatic amino acids by chemiluminometric assay with Luminol-H2O2-Cu(II) system (Luminol-H2O2-Cu(II) 시스템을 이용한 방향족 아미노산의 화학발광법적 정량)

  • Kim, Kyung-Min;Kim, Young-Ho;Lee, Sang-Hak
    • Analytical Science and Technology
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    • v.25 no.3
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    • pp.171-177
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    • 2012
  • A determination method of aromatic amino acids such as trytophan (Trp), tyrosine (Tyr), and phenylalanine (Phe) using luminol-$H_2O_2$-Cu(II) system has been presented. In the presence of an aromatic amino acid, the enhanced chemiluminescence (CL) intensity of luminol-$H_2O_2$-Cu(II) system was obtained by forming a complex between Cu(II) and the amino acid. Based on the above phenomenon, a sensitive and fast determination of three aromatic amino acids was performed using the CL method in batch-type detection system. To optimize determination conditions, the kinetic influence of an aromatic amino acid on the luminol-$H_2O_2$-Cu(II) system and the effects of $H_2O_2$ and Cu(II) concentration, pH, and buffers were investigated. Under the optimized conditions, the calibration curve was linear over the range from $1.0{\times}10^{-6}$ to $2.0{\times}10^{-5}\;M$ for Trp, $1.0{\times}10^{-6}$ to $2.0{\times}10^{-5}\;M$ for Try, and $2.0{\times}10^{-6}$ to $2.0{\times}10^{-5}\;M$ for Phe, respectively. In this range, reproducibility (RSD, n = 4) of Trp, Try, and Phe were 3.21%, 2.64%, and 2.48%, respectively. The limit of detection ($3{\sigma}/s$) was calculated to be $6.8{\times}10^{-7}\;M$ for Trp, $5.7{\times}10^{-7}\;M$ for Try, and $9.6{\times}10^{-7}\;M$ for Phe.