• Title/Summary/Keyword: Analytical Validation

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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.