• Title/Summary/Keyword: Analytical validation

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Exposure Assessment of Apple Orchard Workers to the Insecticide Imidacloprid Using Whole Body Dosimetry During Mixing/Loading and Application (전신복장법을 이용한 농약 조제 및 살포 과정 중 살충제 Imidacloprid에 대한 사과 과수원 농작업자의 노출 평가)

  • Lee, Jae Yun;Noh, Hyun Ho;Park, Hyo Kyoung;Jeong, Hye Rim;Jin, Me Jee;Park, Kyung-Hun;Kim, Jeong-Han;Kyung, Kee Sung
    • The Korean Journal of Pesticide Science
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    • v.20 no.3
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    • pp.271-279
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    • 2016
  • To evaluate exposure characteristics of the insecticide imidacloprid to apple orchard workers during treatment on orchard fields and evaluate its potential risk using a whole body dosimetry (WBD) method, 1,000-time diluted acephate+imidacloprid 25(20+5)% solutions were sprayed on 10 apple orchard fields in Cheongju with a speed sprayer at a rate of 3,000 L/ha/person, after put on clothes such as inner/outer clothes, personal air pump with a IOM sampler, nitrile glove and mask. Exposure test included mixing, loading and application steps. The test pesticide imidacloprid residues in the collected samples were analyzed with a HPLC-DAD. Recoveries ranged from 81.5 to 108.6% for analytical method validation and from 73.8 to 86.7% for field recovery. Total exposed amounts to mixer/loader and applicator were found to be 0.0014-0.0279% of total applied active ingredient of imidacloprid. Glove exposure of both mixer/loader and applicator was higher than the other parts. Margins of safety of mixer/loader and applicator were calculated to be 97-355 and 46-196, respectively, indicating that exposure risk of imidacloprid to apple orchard workers by spraying with a speed sprayer was very low.

Residual Characteristics of Fluquinconazole and Flusilazole in Tomatoes during Greenhouse Cultivation and Processing (토마토 중 fluquinconazole과 flusilazole의 포장 및 가공에 따른 잔류특성)

  • Noh, Hyun Ho;Lee, Jae Yun;Park, Hyo Kyoung;Jeong, Hye Rim;Jin, Me Jee;Lee, Jung Woo;Jeong, Heon Sang;Lee, Sang Hoon;Kyung, Kee Sung
    • The Korean Journal of Pesticide Science
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    • v.21 no.1
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    • pp.84-89
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    • 2017
  • This study was carried out to investigate residue dissipation of fluquinconazole and flusilazole in field-sprayed tomatoes during greenhouse cultivation and processing. The test pesticide, fluquinconazole+flusilazole 8.5 (7+1.5)% SC, was sprayed onto the tomatoes growing in a greenhouse according to Korea preharvest intervals and then samples were collected on 0 (3 hours after spraying), 1, 3, 5 and 7 days after last application for decline test. For processing test, tomatoes collected at harvest on 5 day after last application were processed to puree and juice. Limits of quantitation of fluquinconazole and flusilazole were 0.005 mg/kg in both tomatoes and their processed products. Recoveries for validation of the analytical methods for fluquinconazole and flusilazole in tomatoes and their processed products ranged from 74.8 to 97.5%. Biological half-lives of fluquinconazole and flusilazole in tomatoes under greenhouse conditions found to be 5.2 and 6.4 days, respectively. Average persistent residue levels of fluquinconazole and flusilazole were 37.34 and 79.53% after washing, 8.95 and 28.75% in filtrates after boiling, 3.58 and 14.66% in puree, and 3.34 and 13.52% in juice, respectively. These results indicated that the test pesticide residues on tomatoes could be largely removed through washing and boiling.

Development of Rapid Analytical Method of Forbidden Medicines in Dietary Supplements Using LC-ESI-Tandem MS (LC-ESI-tandem MS를 이용한 기능성표방식품 중 부정유해물질 신속검사체계 개발)

  • Kim, Hee-Yun;Jang, Young-Mi;Joo, Hyun-Jin;Jung, Young-Hyun;Lee, Myoung-Sook;Park, Jong-Seok;Lee, Kwang-Ho;Lee, Hwa-Mi
    • Korean Journal of Food Science and Technology
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    • v.39 no.4
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    • pp.372-379
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    • 2007
  • A high-performance liquid chromatography-electrospray ionization (HPLC-ESI) tandem MS was developed for the rapid and simultaneous determination of forbidden medicines in dietary supplements. Thirteen medicinal components such as PDE-5 inhibitors and their analogues, and the newly identified dimethylsildenafil and xanthoanthrafil, were included in this study. After tentative standardization of molecular ions in both polarities using thirteen references on the mass spectrometer, with ESI-continuous infusion via the syringe pump method, the relative intensity of the ions present in the resulting spectra was quantitatively compared. From the results, the ion mode was selected depending on each reference's characteristics. A HPLC method coupled with the ESI mode was developed considering the matrix effect and interference depending on the type of sample. The validation test of the developed method was followed by carrying out precision, accuracy, recovery, sensitivity and linearity, etc. The method showed sufficiently high sensitivity, reproducibility, and specificity, and produced 4 times faster results when compared with the existing HPLC/UV method for the determination of forbidden compounds in dietary supplements.

An Investigation on Expanding Co-occurrence Criteria in Association Rule Mining (연관규칙 마이닝에서의 동시성 기준 확장에 대한 연구)

  • Kim, Mi-Sung;Kim, Nam-Gyu;Ahn, Jae-Hyeon
    • Journal of Intelligence and Information Systems
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    • v.18 no.1
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    • pp.23-38
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    • 2012
  • There is a large difference between purchasing patterns in an online shopping mall and in an offline market. This difference may be caused mainly by the difference in accessibility of online and offline markets. It means that an interval between the initial purchasing decision and its realization appears to be relatively short in an online shopping mall, because a customer can make an order immediately. Because of the short interval between a purchasing decision and its realization, an online shopping mall transaction usually contains fewer items than that of an offline market. In an offline market, customers usually keep some items in mind and buy them all at once a few days after deciding to buy them, instead of buying each item individually and immediately. On the contrary, more than 70% of online shopping mall transactions contain only one item. This statistic implies that traditional data mining techniques cannot be directly applied to online market analysis, because hardly any association rules can survive with an acceptable level of Support because of too many Null Transactions. Most market basket analyses on online shopping mall transactions, therefore, have been performed by expanding the co-occurrence criteria of traditional association rule mining. While the traditional co-occurrence criteria defines items purchased in one transaction as concurrently purchased items, the expanded co-occurrence criteria regards items purchased by a customer during some predefined period (e.g., a day) as concurrently purchased items. In studies using expanded co-occurrence criteria, however, the criteria has been defined arbitrarily by researchers without any theoretical grounds or agreement. The lack of clear grounds of adopting a certain co-occurrence criteria degrades the reliability of the analytical results. Moreover, it is hard to derive new meaningful findings by combining the outcomes of previous individual studies. In this paper, we attempt to compare expanded co-occurrence criteria and propose a guideline for selecting an appropriate one. First of all, we compare the accuracy of association rules discovered according to various co-occurrence criteria. By doing this experiment we expect that we can provide a guideline for selecting appropriate co-occurrence criteria that corresponds to the purpose of the analysis. Additionally, we will perform similar experiments with several groups of customers that are segmented by each customer's average duration between orders. By this experiment, we attempt to discover the relationship between the optimal co-occurrence criteria and the customer's average duration between orders. Finally, by a series of experiments, we expect that we can provide basic guidelines for developing customized recommendation systems. Our experiments use a real dataset acquired from one of the largest internet shopping malls in Korea. We use 66,278 transactions of 3,847 customers conducted during the last two years. Overall results show that the accuracy of association rules of frequent shoppers (whose average duration between orders is relatively short) is higher than that of causal shoppers. In addition we discover that with frequent shoppers, the accuracy of association rules appears very high when the co-occurrence criteria of the training set corresponds to the validation set (i.e., target set). It implies that the co-occurrence criteria of frequent shoppers should be set according to the application purpose period. For example, an analyzer should use a day as a co-occurrence criterion if he/she wants to offer a coupon valid only for a day to potential customers who will use the coupon. On the contrary, an analyzer should use a month as a co-occurrence criterion if he/she wants to publish a coupon book that can be used for a month. In the case of causal shoppers, the accuracy of association rules appears to not be affected by the period of the application purposes. The accuracy of the causal shoppers' association rules becomes higher when the longer co-occurrence criterion has been adopted. It implies that an analyzer has to set the co-occurrence criterion for as long as possible, regardless of the application purpose period.

Simultaneous Determination of Penicillin Antibiotics in Meat using Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS를 이용한 육류 중 페니실린계 항생제 8종의 동시분석 및 적용성 검증)

  • Kim, Myeong-Ae;Yoon, Su-Jin;Kim, MeeKyung;Cho, Yoon-Jae;Choi, Sun-Ju;Chang, Moon-Ik;Lee, Sang-Mok;Kim, Hee-Jeong;Jeong, Jiyoon;Rhee, Gyu-Seek;Lee, Sang-Jae
    • Journal of Food Hygiene and Safety
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    • v.29 no.2
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    • pp.131-140
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    • 2014
  • The objective of this study was to develop a simultaneous method of 8 penicillin antibiotics including amoxicillin, ampicillin, cloxacillin, dicloxacillin, nafcillin, oxacillin, penicillin G and penicillin V in meat using LC-MS/MS. The procedure involves solid phase extraction with HLB cartridge and subsequent analysis by LC-MS/MS. To optimize MS analytical condition of 8 compounds, each parameter was established by multiple reaction monitoring in positive ion mode. The chromatographic separation was achieved on a $C_{18}$ column with a mobile phase of 0.05% formic acid and 0.05% formic acid in acetonitrile at a flow rate of 0.2 mL/min for 20 min with a gradient elution. The developed method was validated for specificity, linearity, accuracy and precision in beef, pork and chicken. The recoveries were 71.0~106%, and relative standard deviations (RSD) were 4.0~11.2%. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.003~0.008 mg/kg and 0.01~0.03 mg/kg, respectively, that are below maximum residue limit (MRL) of the penicillins. This study also performed survey of residual penicillin antibiotics for 193 samples of beef, pork and chicken collected from 9 cities in Korea. Penicillins were not found in all the samples except a sample of pork which contained cloxacillin (concentration of 0.08 mg/kg) below the MRL (0.3 mg/kg).

A Study on Phthalate Analysis of Nail Related Products (네일 관련 제품들의 프탈레이트 분석에 관한 연구)

  • Rark, Sin-Hee;Song, Seo-Hyeon;Kim, Hyun-Joo;Cho, Youn-Sik;Kim, Ae-Ran;Kim, Beom-Ho;Hong, Mi-Yeun;Park, Sang-Hyun;Yoon, Mi-Hye
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.45 no.3
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    • pp.217-224
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    • 2019
  • Phthalates, endocrine disrupting chemicals, are similar in structure to sex hormones and mainly show reproductive toxicity and developmental toxicity. In this study, we analyzed 11 phthalates, including 3 kinds of phthalates prohibited in cosmetic use and 8 kinds of phthalates regulated in 'Common standards for children's products safety' and EU cosmetic regulation (EC No. 1223/2009). The phthalate analysis was optimized using GC-MS/MS. In analytical method validation, this method was satisfied in specificity, linearity, recovery rate, accuracy and MQL. Therefore, we used this method to analyze 82 products of Nail cosmetics & polish. Although six phthalates such as DBP, BBP, DEHP, DPP, DIBP and DIDP were detected at concentrations of $1.0{\sim}59.8{\mu}g/g$g, they were suitable to Korean cosmetic standards. DIBP and DBP were detected at concentration of $1.1{\sim}2.6{\mu}g/g$ in artificial nail, DBP and DEHP were $1.4{\sim}2.5{\mu}g/g$ in glue for nails, and DIBP, DBP, and DEHP were $2.5{\sim}33.3{\mu}g/g$ in nail stickers. Although substances such as DBP and DEHP in artificial nail, Glue for nails, and nail stickers were detected, they were suitable to 'Common safety standards for children's products. DIBP is not a regulated substance in Korea but showed the third highest detection rate following DBP (84.6%) and DEHP (63.4%). The concentration of phthalates detected in nail products is considered to be safe in current standards but continuous monitoring and research about non-regulated substances are also needed to be considered.

Development of Method using LC-ESI-MS/MS and KASP for Identification of Gymnema sylvestre in Food (식품에서 당살초 판별을 위한 LC-ESI-MS/MS 분석법과 KASP 마커 개발)

  • Park, Boreum;Lee, Sun Hee;Eom, Kwonyong;Noh, Eunyoung;Moon Han, Kyoung;Hwang, Jinwoo;Kim, Hyungil;Baek, Sun Young
    • Journal of Food Hygiene and Safety
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    • v.37 no.2
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    • pp.46-54
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    • 2022
  • Known for its effectiveness in weight loss and diabetes prevention, Gymnema sylvestre products can be found in the US, Japanese, and Indian markets. However, the recommended dosage or safety of these products has not yet been proven. Therefore, development of an analytical method for detecting the content of Gymnema sylvestre in food products is required. Accordingly, this study proposes an analysis method that can examine Gymnema sylvestre in food using LC-ESI-MS/MS and KASP (Kompetitive Allele-Specific PCR) markers. In LC-ESI-MS/MS, a simultaneous analysis method for gymnemic acid and deacylgymnemic acid was optimized using negative ionization mode, and its validation test was completed for solid and liquid samples. In addition, KASP markers were prepared by finding the specific SNP of G. sylvestre in ITS2 and matK through DNA barcodes. The two KASP markers returned positive FAM fluorescence result when combined with G. sylvestre, and this aspect was confirmed in raw G. sylvestre as well. The applicability of the method was tested on 21 different food and healthy functional products containing G. sylvestre purchased on the internet. As a result, although there was a difference in the ratios of gymnemic acid and deacylgymnemic acid in LC-ESI-MS/MS, the index component was detected in all 21 products samples. In the KASP analysis, 9 products returned positive FAM result, and the rest of the products were found to be containing G. sylvestre extract. This study is the first study to use the dual system of LC-ESI-MS/MS and KASP for the analysis of G. sylvestre. The study has confirmed that these two methods are applicable to the examine G. sylvestre content in food products.

Effect of the Suicide Prevention Program to the Impulsive Psychology of the Elementary School Student (자살예방 프로그램이 초등학교 충동심리에 미치는 영향)

  • Kang, Soo Jin;Kang, Ho Jung;Cho, Won Cheol;Lee, Tae Shik
    • Journal of Korean Society of Disaster and Security
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    • v.6 no.1
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    • pp.65-72
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    • 2013
  • In this study, the early suicide prevention program was applied to the elementary school students and compared the prior & post effect of the program, and verified the status of psychology change like emotional status, or temptation to take a suicide, and presented the possibility as a suicide prevention program. The period of adolescence is the very unstable period in the process of growth being cognitively immature, emotionally impulsive period. It is the period emotionally unstable and unpredictable possible to select the method of suicide as an extreme method to escape the reality, or impulsive problem solving against small conflict or dispute situation. Many stress of the student such as recent nuclear family, expectation of parents to their children, education problem, socio-environmental elements, individual psychological factor lead students to the extreme activity of suicide in recent days. In this study, the scope of stress experienced in the elementary school as well as idea and degree of temptation regarding suicide by the suicide prevention program were identified, and through prevention program such as meditation training, breath training and through experience of anger control, emotion-expression, self overcome and establish positive self-identity and make understanding Self-control, Self-esteem & preciousness of life based on which the effect to suicide prevention was analyzed. The study was made targeting 51 students of 2 classes of 6th grade of elementary school of Goyang-si and processed 30 minutes every morning focused on through experience & activity of the principle & method of brain science. The data was collected for 20 times before starting morning class by using Suicide Probability Scale(herein SPS-A) designed to predict effectively suicide Probability, suicide risk prediction scale, surveyed by 7 areas such as Positive outlook, Within the family closeness, Impulsivity, Interpersonal hostility, Hopelessness, Hopelessness syndrome, suicide accident. Analytical methods and validation was used the Wilcoxon's signed rank test using SPSS Program. Though the process of program in short period, but there was a effective and positive results in the 7 areas in the average comparison. But in the t-test result, there was a different outcome. It indicated changes in the 3 questionnaires (No.7, No.14, No.19) out of 31 SPS-A questionnaires, and there was a no change to the rest item. It also indicated more changes of the students in the class A than class B. And in case of the class A students, psychological changes were verified in the areas of Hopelessness syndrome, suicide accident among 7 areas after the program was processed. Through this study, it could be verified that different results could be derived depending on the Student tendency, program professional(teacher in charge, processing lecturer). The suicide prevention program presented in this article can be a help in learning and suicide prevention with consistent systematization, activation through emotion and impulse control based on emotional stress relief and positive self-identity recovery, stabilization of brain waves, and let the short period program not to be died out but to be continued connecting from childhood to adolescence capable to make surrounding environment for spiritual, physical healthy growth for which this could be an effective program for suicide prevention of the social problem.