• Title/Summary/Keyword: sample recovery

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Method of Nitrate Nitrogen Determination for Plant, Soil and Water Analysis by E. coil Cells (E. coli 세포(細胞)를 이용한 식물(植物), 토양(土壤) 및 수질(水質)의 질산태(窒酸態) 질소(窒素) 분석방법(分析方法))

  • Sohn, Sang Mok;Kucke, Martin;Lee, Yoon Gun
    • Korean Journal of Soil Science and Fertilizer
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    • v.30 no.4
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    • pp.361-369
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    • 1997
  • A microbiological nitrate determination method by E. coli is modified in Korea, using K12 wildtype, KCTC 1116, for the quantitative reduction of $NO_3{^-}$ to $NO_2{^-}$. The nitrate in plant, soil or water sample is determined spectrophotometrically after being diazotized with sulfaniamide and N-(1-naphthl)-ethlenediamine. The modified E. coli cell method and principle for nitrate determination using Korean wildtype E. coli strain is described, and cell culture and preparation of stock suspension for E. coli as well. This modified E. coli cell method can be managed simply and fast, it is suitable for the investigation of the large serials, it can be also automated and has a high degree of sensitivity up to 0.01ppm $NO_3{^-}-N$ in the sample solution. The applicability of the modified E. coli cell method has been tested for plant, soil and water analysis on a wide range of different samples. Recovery rates of added nitrate have been determined and comparisons with other standard nitrate analytical procedures have been carried out. The results with the modified E. coli cell method show high correlation ($r^2=0.98$) with those gained by the standard analytical procedures. The advantages and disadvantages of the method are also discussed to other nitrate determination methods.

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Studies on Silk Textile Wash and Wear Finishing (絹織物 Wash and Wear 加工硏究)

  • Choe, Byong-Hee;Lee, Yang-Hoo
    • Journal of Sericultural and Entomological Science
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    • v.23 no.1
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    • pp.47-55
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    • 1981
  • Silk textile finishing has been studied for many years by many workers in order to meet more utilities for various endusers. Such studies, however, could not be successful because any natural fibers are hardly change their natures by artificial treating methods. Textile finishing is of course to improve the mechandise qualities and the poor natures of silk so that it may be available as the best textile fiber in the world. Sometimes, famous trade marked textile plays more power than its quality in the silk market, nevertheless, this should be over line of research activities. Meantime, the silk demand has been also transferred from ladies stocking to other clothes since nylon or other synthetic fibers were developed. That is why, the extension of silk demand should be developed by various research works. Specially, silk is known as difficult textile to handle it during washing or ironing process which happened to depress down the silk usage for house wives. In order to solve such problems, the reporter has been worked for many years and now, he believes that he has developed a proper finishing method to coversuch problems. The developed finishing method may be said to eligible with economical aspect and shorten the dry duration after water washing in half against normal silk textile without harming the specific silk nature. As all of us know, silk fiber starts to denature since it was spinned by silkworm and the fiber is formed as overlapped "S" type curves during its concooning process. After it is made as raw silk or sericin silk, it shows as straight line form, but it changes in to waved form in case refining or degumming process in order return to its original spinned form. Such nature is continued during its textile form and ends with hard ironing nature than other textile fibers. Mean while, the silk fiber keeps to continue its denaturing and this is iniciated by repeat of washing and drying which takes many years to reach its final stage, The reporter has found the iniciating denature of silk by his finishing process, with out heat, decreasing the swollen nature which ended with shortening the drying duration after wash. Each washing was carried out by soaking the previously weighed sample in cold water for one hour, then pressed the sample for ten minutes to eliminate its free water component before weighing with same condition. According to this, the treated silk showed much denaturing after the finishing, but the standard silk progressed the denaturing by and by with the repeat of washing and drying, finally reached the same swollen degree of treated silk, Such treating result explains that the treated silk happened to be stebilized nature by the treating immediately. On the other that the treated silk happened to be stebilized nature by the treating immediately. On the other hand, standard silk may reach to such condition by the time of worn out clothes after repeat of washing and drying for many years while the clothes will be no more useful. The decreased swelling nature has brought about the drying period in half against standard silk after all. Not only the tests of tenacity and elongation but also crease resistance recovery, stiffness and shrinkage tests were carried out after each washing and drying which he has found better result on the treated silk textile against the standard silk. The most important thing was to keep the textile feeling of silk by such finishing work before improve any poor nature of silk. The general silk has a nature to absorb smoke or dirt from its surrounding air and reaches to dirty color shade upon such exposure, but the treated one has improved such nature because of its artificial denaturing, another word, it keeps clean longer than the normal silk. Many previous finishing works could improve some specific nature of silk, but it happened to deprave other important natures. The reporters work is, however, specialized to improve the silk to be useful as Wash and Wear Silk without harming its standard natures. So far, this work happened to be a overall innovative finishing method of silk textile.

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Single Laboratory Validation and Uncertainty Estimation of a HPLC Analysis Method for Deoxynivalenol in Noodles (면류에서 HPLC를 이용한 데옥시니발레놀 분석법의 검증과 불확도 산정)

  • Ee, Ok-Hyun;Chang, Hyun-Joo;Kang, Young-Woon;Kim, Mee-Hye;Chun, Hyang-Sook
    • Journal of Food Hygiene and Safety
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    • v.26 no.2
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    • pp.142-149
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    • 2011
  • An isocratic high performance liquid chromatography (HPLC) method for routine analysis of deoxynivalenol in noodles was validated and estimated the measurement uncertainty. Noodles (dried noodle and ramyeon) were analyzed by HPLC-ultraviolet detection using immunoaffinity column for clean-up. The limits of detection (LOD) and quantification (LOQ) were 7.5 ${\mu}g$/kg and 18.8 ${\mu}g$/kg, respectively. The calibration curve showed a good linearity, with correlation coefficients $r^2$ of 0.9999 in the concentration range from 20 to 500 ${\mu}g$/kg. Recoveries and Repeatabilities expressed as coefficients of variation (CV) spiked with 200 and 500 ${\mu}g$/kg were $82{\pm}2.7%$ and $87{\pm}1.3%$% in dried noodle, and $97{\pm}1.6%$ and $91{\pm}12.0%$ in ramyeon, respectively. The uncertainty sources in measurement process were identified as sample weight, final volume, and sample concentration in extraction volume as well as components such as standard stock solution, working standard solution, 5 standard solutions, calibration curve, matrix, and instrument. Deoxynivalenol concentration and expanded uncertainty in two matrixes spiked with 200 ${\mu}g$/kg and 500 ${\mu}g$/kg were estimated to be $163.8{\pm}52.1$ and $435.2{\pm}91.6\;{\mu}g$/kg for dried noodle, and $194.3{\pm}33.0$ and $453.2{\pm}91.1\;{\mu}g$/kg for ramyeon using a coverage factor of two which gives a level of statistical confidence with approximately 95%. The most influential component among uncertainty sources was the recovery of matrix, followed by calibration curve.

Analysis of 236 Pesticides in Apple for Validation of Multiresidue Method using QuEChERS Sample Preparation and PTV-GC/TOFMS Analysis (QuEChERS법과 PTV-GC/TOFMS 이용 잔류농약 분석법 개발을 위한 사과시료 중 236종 농약의 동시분석)

  • Ju, Ok-Jung;Kwon, Hye-Young;Park, Byeong-Jun;Kim, Chan-Seob;Jin, Yong-Duk;Lee, Je-Bong;Yun, Seo-Hee;Son, Kyung-Ae;Hong, Su-Myeong;Im, Geon-Jae
    • The Korean Journal of Pesticide Science
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    • v.15 no.4
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    • pp.401-416
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    • 2011
  • The recent trend for pesticide residue analysis in food involves fast cleanup and use of mass spectrometry to achieve quantitative and qualitative analysis at the same time. Recently, the QuEChERS (quick, easy, cheap, effective, rugged and safe) multi-reside method has received much attention as a fast extraction and cleanup method of pesticide residue analysis. Therefore, multi-residue analysis of 236 pesticides was tested with the QuEChERS method by concurrent use of PTV-GC/TOFMS (gas chromatography/ time-of-flight mass spectrometry with programmable temperature vaporizer). PTV condition was optimized and when the method was applied to apples, pesticide recovery rates (spiked at 400 ng/g) ranged from 80% to 120%, and RSD values were under 10% for most compounds. The results showed that the QuEChERS sample preparation and PTV-GC/TOFMS analysis can be applied to multi-residue analysis of pesticides in fruits and vegetables.

National Survey of Injury and Poisoning on a Representative Sample Population of Koreans (우리나라 대표적(代表的) 표본인구(標本人口)의 연간(年間) 손상(損傷) 및 중독발생율(中毒發生率)과 역학적(疫學的) 특성(特性))

  • Kim, Joung-Soon;Kim, Sung-Soo;Chang, Sung-Chill
    • Journal of Preventive Medicine and Public Health
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    • v.27 no.3 s.47
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    • pp.447-463
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    • 1994
  • Despite the public health importance of injury and poisoning in terms of its high mortality and incidence, epidemiologic information to be utilized are scarce in Korea. This study was carried out in 1990 on a representative sample population (about 55,000 persons) along with the 6th National Tuberculosis Prevalence Survey in order to estimate the magnitude of injury and poisoning occurrence and to identify its epidemiologic characteristics which can be aided for establishing preventive strategy. Pre-tested and structured Questionnaire was used by trained interviewer to collect data including general information of the person, various information on the injury and poisoning during the past one year such as time and place of its occurrence, its nature and external causes, type of medical institute attended, duration of treatment and outcome of the accident occured. In analysis of the data collected incidence rates per 1000 persons by sex, age group and its nature as well as external causes, and relative frequencies were calculated. The result obtained are as followings; 1. The incidence rate per 1000 was 30 for both sexes, 39 for male and 22 for female, male being 1.8 times more frequent than female. Age adjusted incidences were not much different from the crude rates. Age group specific rate curve showed bimodal shape in both sexes, small peaks in preschool children and higher peaks in older ages. The incidence rate per 1000 people by area was highest in Jeon-bug province (57/1000) and the lowest in Daegu city(11/1000). 2. The place where the injuries occured were road in 46%, within the boundary of house in 25%, and working place in 12% The injuries and poisoning had occured more frequently during the months from March to August of the year than other months. 3. The relatively frequent injuries by its nature were contusion with intact skin surface (19%), fracture of upper limb (13%), open wound of head, neck and trunk (12%) and fracture of lower limb (11%) among males; contusion with intact skin surface (28%), sprains and strains of joints and adjacent muscle (14%), fracture of upper limb (10%) and fracture of lower limb (9%) among females. Higher incidence rate among males than females were fracture of skull (4.5 times), open wound and fractures of limbs ($2{\sim}3$ times). Age specific rate of injuries and poisoning by its nature showed increasing pattern by age in fractures of upper and lower limbs and sprains & strains of joints whereas the age group of 30's showed highest incidence in open wounds of upper limb. Fractures of radius and ulna in upper limb, fractures of tibia & fibula and ankle in lower limb were most frequent among fractures of upper and lower limbs. The frequent injuries among sprains and strains of joints and adjacent muscles were that of ankle, foot and back, and among open wound were that of head and fingers. 4. Relative frequency of injuries and poisoning by external causes showed following order : other accidents (25%), accidental falls (23%), motor vehicle accident (22%) and other road vehicle accident (14%) among males and accidental falls (37%), motor vehicle accident (24%) and other accident (18%) among females. The external causes revealing higher incidences among males than females, were other road vehicle accident (4.8 times), vehicle accident not elsewhere classifiable (4.4 times), accidental poisoning (4.4 times), accidents due to natural and environmental factors (2.8 times), and sucide & self-inflicted injuries (2.8 times). Age specific incidence by external causes for frequent injuries showed that incidence of other accident steadily increased from 10's till age 50's; motor vehicle traffic accident increased from age 20's and dropped after age 60's; on the other hand accidental fall increased strikingly by age. The most frequent external causes among motor vehicle traffic accidents was motor vehicle traffic accident involving collision with pedstrain (69%), pedal cycle accident (30%) and other road vehicle accident (71%) among other road vehicle accidents; falls on same level from slipping, tripping or standing (44%) and other falls from one level to another among accidental falls; accidents caused by machinary (32%) for male and striking against or struck accidentally by objects or person for female among other accidents. 5. Seventy nine percent of the injuries and poisonings were treated in general hospital or hospital/clinic. The duration of treatment ranged from a few days to 123 weeks; the majority(52%) took under 2 weeks, 36% for $3{\sim}8$ weeks and 4% over 21 weeks. 6. The accident resulted in full recovery of normal healthy state in 62%, residual functional defects in 21% and on process of treatment in 16%.

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Development of simultaneous analytical method for investigation of ketamine and dexmedetomidine in feed (사료 내 케타민과 덱스메데토미딘의 잔류조사를 위한 동시분석법 개발)

  • Chae, Hyun-young;Park, Hyejin;Seo, Hyung-Ju;Jang, Su-nyeong;Lee, Seung Hwa;Jeong, Min-Hee;Cho, Hyunjeong;Hong, Seong-Hee;Na, Tae Woong
    • Analytical Science and Technology
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    • v.35 no.3
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    • pp.136-142
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    • 2022
  • According to media reports, the carcasses of euthanized abandoned dogs were processed at high temperature and pressure to make powder, and then used as feed materials (meat and bone meal), raising the possibility of residuals in the feed of the anesthetic ketamine and dexmedetomidine used for euthanasia. Therefore, a simultaneous analysis method using QuEChERS combined with high-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry was developed for rapid residue analysis. The method developed in this study exhibited linearity of 0.999 and higher. Selectivity was evaluated by analyzing blank and spiked samples at the limit of quantification. The MRM chromatograms of blank samples were compared with those of spiked samples with the analyte, and there were no interferences at the respective retention times of ketamine and dexmedetomidine. The detection and quantitation limits of the instrument were 0.6 ㎍/L and 2 ㎍/L, respectively. The limit of quantitation for the method was 10 ㎍/kg. The results of the recovery test on meat and bone meal, meat meal, and pet food showed ketamine in the range of 80.48-98.63 % with less than 5.00 % RSD, and dexmedetomidine in the range of 72.75-93.00 % with less than 4.83 % RSD. As a result of collecting and analyzing six feeds, such as meat and bone meal, prepared at the time the raw material was distributed, 10.8 ㎍/kg of ketamine was detected in one sample of meat and bone meal, while dexmedetomidine was found to have a concentration below the limit of quantitation. It was confirmed that the detected sample was distributed before the safety issue was known, and thereafter, all the meat and bone meal made with the carcasses of euthanized abandoned dogs was recalled and completely discarded. To ensure the safety of the meat and bone meal, 32 samples of the meat and bone meal as well as compound feed were collected, and additional residue investigations were conducted for ketamine and dexmedetomidine. As a result of the analysis, no component was detected. However, through this investigation, it was confirmed that some animal drugs, such as anesthetics, can remain without decomposition even at high temperature and pressure; therefore, there is a need for further investigation of other potentially hazardous substances not controlled in the feed.

Vitamin D analysis in the Korean total diet study and UV/sun light irradiated mushrooms (한국형 총식이조사 및 UV/태양광 조사 버섯에서의 비타민 D 분석)

  • Min-Jeong Seo;In-Hwa Roh;Jee-Yeon Lee;Sung-Ok Kwon;Cho-Il Kim;Gae-Ho Lee
    • Food Science and Preservation
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    • v.30 no.1
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    • pp.109-121
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    • 2023
  • This study was conducted to evaluate vitamin D intake of Koreans in a total diet study (TDS) and to determine the effect of irradiation on vitamin D synthesis in mushrooms. For analysis, sample were saponified and extracted with hexane, and vitamin D was quantified by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Based on the validation results, the recovery of the National Institute of Standards and Technology (NIST) standard reference sample (SRM) 1849a was 96.7% and the z-score of -1.6 was obtained by the Food Analysis Performance Assessment Scheme (FAPAS) proficiency test (PT) 21115. Vitamin D2 was not detected in any samples, and the highest level of vitamin D3 was detected in mackerel and anchovies ranging from 24.2 to 120.2 ㎍/kg. The mean daily intake of vitamin D was 0.99 ㎍/day, as estimated from the vitamin D contents of the analyzed foods and their corresponding intake. The adequate intake (AI) of vitamin D based on the Dietary reference intakes for Koreans provided by the Ministry of Health and Welfare is 5-15 ㎍/day for Koreans aged 6 to 75 years. Compared with this AI, vitamin D intake of Koreans estimated in this study was inadequate. For that, the increased vitamin D content in ultraviolet (UV)/sun light irradiated mushrooms warrants further research to increase vitamin D intake of Koreans through diet.

Development of a Simultaneous Analytical Method for Determination of Insecticide Broflanilide and Its Metabolite Residues in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살충제 Broflanilide 및 대사물질 동시시험법 개발)

  • Park, Ji-Su;Do, Jung-Ah;Lee, Han Sol;Park, Shin-min;Cho, Sung Min;Kim, Ji-Young;Shin, Hye-Sun;Jang, Dong Eun;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.124-134
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    • 2019
  • An analytical method was developed for the determination of broflanilide and its metabolites in agricultural products. Sample preparation was conducted using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method and LC-MS/MS (liquid chromatograph-tandem mass spectrometer). The analytes were extracted with acetonitrile and cleaned up using d-SPE (dispersive solid phase extraction) sorbents such as anhydrous magnesium sulfate, primary secondary amine (PSA) and octadecyl ($C_{18}$). The limit of detection (LOD) and quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. The recovery results for broflanilide, DM-8007 and S(PFP-OH)-8007 ranged between 90.7 to 113.7%, 88.2 to 109.7% and 79.8 to 97.8% at different concentration levels (LOQ, 10LOQ, 50LOQ) with relative standard deviation (RSD) less than 8.8%. The inter-laboratory study recovery results for broflanilide and DM-8007 and S (PFP-OH)-8007 ranged between 86.3 to 109.1%, 87.8 to 109.7% and 78.8 to 102.1%, and RSD values were also below 21%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food and Drug Safety Evaluation guidelines (2016). Therefore, the proposed analytical method was accurate, effective and sensitive for broflanilide determination in agricultural commodities.

EVALUATION OF SERUM LEVELS OF SYSTEMIC STATUS IN ORAL AND MAXILLOFACIAL SURGERY PATIENTS (구강악안면 수술을 받은 환자들에서의 전신영양평가)

  • Kim, Uk-Kyu;Kim, Yong-Deok;Byun, June-Ho;Shin, Sang-Hun;Chung, In-Kyo
    • Journal of the Korean Association of Oral and Maxillofacial Surgeons
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    • v.29 no.5
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    • pp.301-314
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    • 2003
  • The purposes of this retrospective study were to assess the change of serum parameters in oral and maxillofacial surgery patients after operation and to determine what laboratory parameters on treatment periods were associated with the recovery of systemic condition. For purposes of assessing systemic nutritional status, several serum parameters were chosen. The sample patients were randomsubjects extracted from three category patient groups- oral cancer, odontogenic abscess, facial bone fracture based on treated patients at department of oral and maxillofacial surgery in Pusan National University Hospital from September 1, 1998, to September 1, 2002. Each groups were consisted with 10 patients. Each patient chart was examined and blood sample parameters were reviewed with clinical signs, symptoms and vital sign at preoperative day, postoperative 1 day, postoperative 1 week. Several parameters were analyzed statistically for extraction of mean values and differences between the periods groups. The findings of serum parameters of cancer, abscess and fracture groups were as follows: 1. In cancer patients, Hb, MCV, albumin, cholesterol, LDH, AST, ALT, neutrophil, platelet, leukocyte, Na, K, Cl, BUN, creatinine were analyzed. Values of Hb, albumin, AST, neutrophil, leukocyte, Cl showed significantly differences according to periods. 2. In abscess patients, CRP, ESR, leukocyte, body temperature, neutrophil were analyzed. Values of CRP, leukocyte, body temperature, neutrophil showed significanlty differences according to periods. 3. In fracture patients, same parameters with cancer patient's were chosen. Values of platelet, Cl only showed significantly differences according to periods. 4. In cancer patients, data regarding correlation was analyzed statistically as Pearson's value. A positive correlation was found between Hb and albumin, K, Na(P<0.05). A positive correlation was also found between neutrophil and leukocyte(P<0.05). Positive correlations were found between cholesterol and ALT, LDH and platelet, creatinine both, Platelet and BUN, Na and K(P<0.01). 5. In abscess patients, Peason's correlation values were analyzed on parameters. A positive correlation was found only between CRP and neutrophil(P<0.05). 6. In fracture patients, The correlations of parameters also were statistically analyzed. Positive correlations were found between MCV and K, albumin and LDH, AST and three parameters of creatinine, Na, Cl, K and neutrophil, neutrophil and three parameters of leukocyte, BUN, K(P<0.05). Positive correlations were found between LDH and AST, ALT and AST, creatinine both(P<0.01). This retrospective clinical study showed the CRP levels only on abscess patients may be useful in determination of clinical infected status, but the levels of other parameters on cancer, fracture patients did not showed significant values as diagnostic aids for clinical status.

Translocation of Tolclofos-methyl from Ginseng Cultivated Soil to Ginseng (Panax ginseng C. A. Meyer) and Residue Analysis of Various Pesticides in Ginseng and Soil (토양 중 잔류된 Tolclofos-methyl의 인삼(Panax ginseng C. A. Meyer)에 대한 이행 및 잔류 특성)

  • Kim, Ji Yoon;Kim, Hea Na;Saravanan, Manoharan;Heo, Seong Jin;Jeong, Haet Nim;Kim, Jang Eok;Kim, Kwan Rae;Hur, Jang Hyun
    • The Korean Journal of Pesticide Science
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    • v.18 no.3
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    • pp.130-140
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    • 2014
  • Recently, some of the previous studies reported that tolclofos-methyl is still exist in ginseng cultivated soil, even though it is has been banned for ginseng. Therefore, the current study was aimed to examine the levels of absorption and translocation of tolclofos-methyl from ginseng cultivated soil to ginseng root and leaf stem for the period of 1 year. For this study, ginseng plants were transplanted in pots and treated with $5.0mg\;kg^{-1}$ of tolclofos-methyl (50% WP). At the end of each interval periods (every three months) the samples (soil, roots and leaf stems) were collected and analyzed the absorption and translocation levels of tolclofos-methyl using gas chromatography and mass spectrometry (GC-MS). The limit of quantitation of tolclofos-methyl was found to be $0.02mg\;kg^{-1}$ and 70.0~120.0% recovery was obtained with coefficient of variation of less than 10% regardless of sample types. In this study, a considerable amount of translocation of tolclofos-methyl residues were found in soil (4.28 to $0.06mg\;kg^{-1}$), root (7.09 to $1.54mg\;kg^{-1}$) and leaf stem (0.79 to $0.69mg\;kg^{-1}$). The results show that the tolclofos-methyl was absorbted and translocated from ginseng cultivated soil to ginseng root and ginseng leaf stem and found to be decreased time-coursely. Secondly, we were also analyzed soil, root and leaf stems samples from Hongcheon, Cheorwon, Punggi and Geumsan by GC-MS/MS (172 pesticides), LC-MS/MS (74 pesticides). In this study, 43 different pesticides were detected ($0.01{\sim}7.56mg\;kg^{-1}$) in soil, root and leaf stem. Further, tolclofos-methyl was detected 4 times separately in root sample alone which is less ($0.01{\sim}0.05mg\;kg^{-1}$) than their maximum residual limit (MRL) in ginseng. Consequently, the results from both studies indicate the residues of tolclofos-methyl found in ginseng cultivated soil and ginseng ensuring their safety level. Moreover, long-term evaluations are needed in order to protect the soil as well as ginseng free from tolclofos-methyl residues.