• Title/Summary/Keyword: 표준적합성 시험

Search Result 291, Processing Time 0.03 seconds

Development and Validation of an Analytical Method for Quinoxyfen in Agricultural Products using QuEChERS and LC-MS/MS (QuEChERS법 및 LC-MS/MS를 이용한 농산물 중 살균제 Quinoxyfen의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Choi, Young-Nae;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
    • /
    • v.34 no.2
    • /
    • pp.140-147
    • /
    • 2019
  • An analytical method was developed for the determination of quinoxyfen in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with 1% acetic acid in acetonitrile and water was removed by liquid-liquid partitioning with $MgSO_4$ (anhydrous magnesium sulfate) and sodium acetate. Dispersive solid-phase extraction (d-SPE) cleanup was carried out using $MgSO_4$, PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed by using LC-MS/MS in positive mode with MRM (multiple reaction monitoring). The matrix-matched calibration curves were constructed using six levels ($0.001-0.25{\mu}g/mL$) and the coefficient of determination ($R^2$) was above 0.99. Recovery results at three concentrations (LOQ, 10 LOQ, and 50 LOQ, n=5) were in the range of 73.5-86.7% with RSDs (relative standard deviations) of less than 8.9%. For inter-laboratory validation, the average recovery was 77.2-95.4% and the CV (coefficient of variation) was below 14.5%. All results were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for quinoxyfen determination in agricultural commodities. This study could be useful for the safe management of quinoxyfen residues in agricultural products.

Development of a Simultaneous Analytical Method for Azocyclotin, Cyhexatin, and Fenbutatin Oxide Detection in Livestock Products using the LC-MS/MS (LC-MS/MS를 이용한 축산물 중 유기주석계 농약 Azocyclotin, Cyhexatin 및 Fenbutatin oxide의 동시시험법 개발)

  • Nam Young Kim;Eun-Ji Park;So-Ra Park;Jung Mi Lee;Yong Hyun Jung;Hae Jung Yoon
    • Journal of Food Hygiene and Safety
    • /
    • v.38 no.5
    • /
    • pp.361-372
    • /
    • 2023
  • Organotin pesticide is used as an acaricide in agriculture and may contaminate livestock products. This study aims to develop a rapid and straightforward analytical method for detecting organotin pesticides, specifically azocyclotin, cyhexatin, and fenbutatin oxide, in various livestock products, including beef, pork, chicken, egg, and milk, using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The extraction process involved the use of 1% acetic acid in a mixture of acetonitrile and ethyl acetate (1:1). This was followed by the addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium chloride. The extracts were subsequently purified using octadecyl (C18) and primary secondary amine (PSA), after which the supernatant was evaporated. Organotin pesticide recovery ranged from 75.7 to 115.3%, with a coefficient of variation (CV) below 25.3%. The results meet the criteria range of the Codex guidelines (CODEX CAC/GL 40). The analytical method in this study will be invaluable for the analysis of organotin pesticides in livestock products.

Simultaneous determination of 11-nor-Δ9-carboxy-tetrahydrocannabinol and 11-nor-Δ9-carboxy-tetrahydrocannabinol-glucuronide in urine samples by LC-MS/MS and its application to forensic science (LC-MS/MS를 이용한 소변 중 11-nor-Δ9-carboxy-tetrahydrocannabinol 및 11-nor-Δ9-carboxy-tetrahydrocannabinol-glucuronide의 동시 분석 및 법과학적 적용)

  • Park, Meejung;Kim, Sineun
    • Analytical Science and Technology
    • /
    • v.34 no.6
    • /
    • pp.259-266
    • /
    • 2021
  • Cannabis (Marijuana) is one of the most widely used drugs in the world, and its distribution has been controlled in South Korea since 1976. Identification of 11-nor-Δ9-carboxy-tetrahydrocannabinol (THCCOOH) in urine can provide important proof of cannabis use, and it is considered scientific evidence in the forensic field. In this study, we describe a simultaneous quantitative method for identifying THCCOOH and THCCOOH-glucuronide in urine, using simple liquid-liquid extraction (LLE), and liquid chromatography-tandem mass spectrometry (LC-MS/MS). THCCOOH-D3 and THCCOOH-glucuronide-D3 were used as internal standards. Validation results of the matrix effect, as well as recovery, linearity, precision, accuracy, process efficiency, and stability were all satisfactory. No carryover, endogenous or exogenous interferences were observed. The limit of detection (LOD) of THCCOOH and THCCOOH-glucuronide were 0.3 and 0.2 ng/mL, respectively. The developed method was applied to 28 authentic human urine samples that tested positive in immunoassay screening and gas chromatography/mass spectrometry (GC/MS) tests. The ranges of concentrations of THCCOOH and THCCOOH-glucuronide in the samples were less than LOQ~266.90 ng/mL and 6.43~2133.03 ng/mL, respectively. The concentrations of THCCOOH-glucuronide were higher than those of THCCOOH in all samples. This method can be effectively and successfully applied for the confirmation of cannabinoid use in human urine samples in the forensic field.

Development and Interlaboratory Validation of an Analytical Method for the Determination of Saflufenacil in Agricultural Products by HPLC-UVD and LC-MS

  • Do, Jung-Ah;Park, Hyejin;Kwon, Ji-Eun;Oh, Jae-Ho;Cho, Yoon-Jae;Chang, Moon-Ik;Choi, Won-Jo;Lee, Hyun-Sook;Hong, Jin-Hwan
    • Journal of Food Hygiene and Safety
    • /
    • v.29 no.4
    • /
    • pp.285-291
    • /
    • 2014
  • Saflufenacil is a low-volatile and uracil-based herbicide. This herbicide is used for pre-and post-emergence control of major broadleaf weeds. The objective of present study was to develop and validate an analytical method for saflufenacil determination in agricultural products for ensuring the food safety. The saflufenacil residues in samples were extracted with acetone, dichloromethane, and then purified with silica and graphitized carbon cartridge. The purified samples were analyzed by HPLC-UVD and confirmed with LC-MS. The linear range of saflufenacil was $0.1{\sim}5.0{\mu}gmL^{-1}$ with the correlation coefficient (r) = 0.999. Average recoveries of saflufenacil ranged from 80.5% to 110.2% at the spiked level of $0.02{\sim}0.5mgkg^{-1}$, while the relative standard deviation was 0.3~7.3%. In addition, the limit of detection and limit of quantification were 0.005 and $0.02mgL^{-1}$, respectively. Furthermore, an interlaboratory study among three labs was conducted to validate the method, and the results were satisfactory.

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
    • /
    • v.34 no.3
    • /
    • pp.235-241
    • /
    • 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.

(2)건강기능식품법의 하위법 제정에 즈음한 방향 제안

  • Son, Dong-Hwa
    • Bulletin of Food Technology
    • /
    • v.15 no.4
    • /
    • pp.73-101
    • /
    • 2002
  • 21세기는 과학기술의 비약적인 발전으로 정보통신기술, 환경기술, 나노기술 그리고 생명과학에 의한 바이오기술이 고부가가치 지식산업으로서 국가경쟁력 강회를 위한 국가전략 핵심산업으로 대두되고 있습니다. 특히 바이오기술의 응용산업인 건강기능식품은 국민의 질병예방과 건강증진을 통한 삶의 질 향상에 이바지하고, 21세기 미래 고부가가치산업으로 발전할 것으로 기대하고 있습니다. 이러한 시기에 국민보건과 건강기능식품산업의 발전을 위한 건강기능식품에 관한 법률(건강기능식품법) 이 의원입법으로 국회에 상정되어 1년 이상의 검토를 거쳐 지난 7월 31일에 국회 본회의를 통과하였습니다. 그후 8월 26일자로 이 법을 정부에서 공포하였으며 내년 8월 26일부터는 발효할 예정입니다. 그러나, 건강기능식품법의 제정은 건강기능식품관련 제도의 완성이 아니라 시작입니다. 즉, 건강기능식품법의 기초는 마련하였지만, 그 하위법인 시행령, 시행규칙, 고시등이 제대로 된 모습을 갖추어야 비로소 국민이 만족하고, 산학연의 동반 발전을 이룰 수 있는 이 분야의 산업발전을 기할 수 있습니다. 그리고, 건강기능식품담당 정부부처인 식품의약품안전청은 현실적으로 그 하위법을 금년 말(2002년)이나 내년 초(2003년)에 준비한 후 입법 예고하여야하는 시간적 제약을 안고 있습니다. 이러한 연유로 단기간 내에 하위법을 준비하다 보면 자칫 애초에 정부와 산학연이 바라던 바와는 다른 엉뚱한결과를 초래할 우려가 있는 만큼, 법 제도의 명확한 방향설정이 매우 중요합니다. 그래서, 한국식품과학회 건강기능식품분과위원회는 이 문제의 중요성을 깊이 인식하고 산학연 전문가그룹(식품과학자, 영양과학자, 학계, 연구계, 기업계: 16인)을 구성하였습니다. 전문가그룹은 지난 7 - 8월, 2달 동안에 수 차례 회의를 통하여, 건강기능식품법 하위법 준비 중 핵심사항은 건강기능식품의 기능성 표시와 평가 라는 점에 착안하고, 이에 대하여 중점적으로 검토하였습니다. 그 이외에도 섭취량 설정 , 심사자료의 인증요건 , 기능성분의 표시 등에 대하여도 부수적으로 검토하였습니다. 그 결과, 동물실험을 이용한 기능성평가 방향 (이미 본지의 전호에서 게재한 바 있어생략)을 제외한 주요사항을 다음의 별도 기사로 각각 소개합니다. 또한, 이 내용은 지난 9월 13일, COEX에서 제1회 건강기능식품 전시회 및 학술세미나 행사의 일환으로서 개최된 학술세미나에서 발표하고 토론회를 거쳤습니다. 또한, 지난 10월 26일, 무주리조트에서 식품과학회 추계학술대회 행사의 일환으로 개최된 건강기능식품분과위원회의 토론회에서도 좋은 의견을 교환한 바 있습니다. 두 차례의 토론회를 통하여 건강기능식품분과위원회가 제안한 초안이 대체적으로 매우 바람직한 것으로 평가받았으며 많은 동의를 얻었습니다. 이어서 토론회의 내용을 반영한 식품과학회의 안을 최종적으로 준비하고 이를 11월초에 식품의약품안전청에게 정책 건의하였습니다. 다음의 별도기사에 덧붙여서, 토론회를 통하여 수정(또는 강조)하고자 하는 부분은 아래와 같습니다. 1) 동물실험 등에서 흡수, 대사 등으로 표기한 서술 용어는 흡수, 분포, 대사, 배설 로 대체합니다. 2) 기능성 평가방법의 표준화와 관련하여 분과위원회에서 제시한 안은 평가방법은 심의위원회가 사안에 따라 기능성 평가시에 그 평가방법의 적합성을 검토함이 바람직하다 라고 하였습니다. 그러나, 이를 부분적으로는 평가방법을 표준화할 필요가있다 로 수정하고자 합니다. 즉, 평가방법이 전혀 제시되지 않으면 막막함으로, 기본적인 방법이면서 여러사람들이 참고로 할만한 방법에 대하여는 표준화를 병행함이 더욱 좋겠다고 생각합니다. 또한, 표준방법으로 제시된 것만이 유일한 방법은 아니므로 다른 방법으로 평가하는 것도 가능함으로 제시합니다. 3) (가칭)건강기능식품 인체시험 관리지침과 관련하여 이는 식약청장이 정할 사안이지만, 그것은 국내 의약품 임상시험 관리지침 과는 뚜렷이 차별화되는 것으로 실제로는 의사의 도움없이도 인체시험을 시행할 수 있음을 명확히 할 필요가 있습니다.

  • PDF

Analysis of quercetin in extract of Hovenia dulcis Thunb (헛개나무과병추출물 중 퀘르세틴 분석)

  • Hu, SooJung;Oh, Jae-Myoung;Oh, Hyun-Suk;Moon, Myung-Hee;Bae, Yun-Young;Lee, Sung-Hye;Kim, Ji-An;Koo, Yong-Eui
    • Analytical Science and Technology
    • /
    • v.29 no.6
    • /
    • pp.255-260
    • /
    • 2016
  • Based on the Korean Health Functional Food Act, health functional foods are dietary supplements containing nutrients or other substances that have nutritional or physiological effects. Since generic health functional food items have been expanded, this project was performed to develop a standardized analytical method of examining such sale items. The method exhibited high linearity in the quercetin calibration curve ($R^2$ > 0.999) over concentrations of $0-40{\mu}g/mL$. The limits of detection and quantitation for quercetin were $0.12{\mu}g/mL$ and $0.36{\mu}g/mL$, respectively, while quercetin recovery was 97.1-105.4 % with standard deviations of 1.15-3.11 %. To verify the accuracy of the analytical methods, the labeled amounts of purchased health functional foods were monitored. The recovery rate for multiple quercetin concentrations ranged from 82.5-105.1 % of the labeled amounts. Thus, the new method was suitable for all cases.

Proficiency Testing for the Gas-chromatographic Analysis of Procymidone, Chlorpyrifos and Metolachlor Residues in Soil (가스크로마토그래피를 이용한 토양 중 프로사이미돈과 클로르피리포스, 메톨라클로르의 잔류분석 숙련도시험)

  • Kim, Chan-Sub;Son, Kyeong-Ae;Gil, Geun-Hwan;Kim, Jin-Bae;Hong, Su-Myeong;Kwon, Hye-Young
    • The Korean Journal of Pesticide Science
    • /
    • v.17 no.2
    • /
    • pp.94-106
    • /
    • 2013
  • The proficiency testing for the residue laboratories of pesticide registration was conducted in order to improve the reliability and the ability for pesticide residue analysis. On October 2011 the testing was carried out using the soil collected and kept as the moistened state for five years, which is expected to very low residue levels of pesticides. The soil was fortified with chlorpyrifos, metolachlor and procymidone in a manner similar to prepare soil sample for indoor soil degradation test, and then sub-samples were prepared for the distribution to participants. Some of them were randomly selected for confirm of homogeneity and to ensure the stability of samples at room temperature. Samples were consisted of two soil treated as different levels, one of which was used to the assesment and another used to confirm. In addition, provide three standard solutions, respectively concentration of 10 mg/L, and untreated soil. Forty seven institutions submitted results. The medians of results were used as the assigned values for pesticide residues. Fitness for purpose standard deviation of proficiency test was calculated by applying 20% RSD as the coefficient of variation allowed in the soil residue test. Z-score was applied for evaluation of individual pesticides, and the average of the absolute value of the Z-score for the overall assessment of pesticides. Laboratories evaluated the absolute value of the Z-score less than 2 to fit the case of chlorpyrifos and procymidone were 44, metolachlor 40.

Growth Characteristics and Productivity of New Orchardgrass(Dactylis glomerata L.) Variety “Jangbeol 101” (오차드그라스 신품종 “장벌 101호”의 생육특성과 수량성)

  • 임용우;최기준;성병렬;임영철;김맹중;박근제;김기용;정종원;박남건
    • Journal of The Korean Society of Grassland and Forage Science
    • /
    • v.23 no.3
    • /
    • pp.203-206
    • /
    • 2003
  • New orchardgrass(Dactylis glomerata L.) variety named as “Jangbeol 101” was developed by the National Livestock Research Institute(NLRI) in 2002. To develope the new variety of orchardgras, 5 superior clones were selected and polycrossed for seed production. Synthetic seeds were examined on the agronomic growth characteristics and forage production at Suwon from 1995 to 1998, and regional trials were conducted in Suwon, Namwon and Pyungchang from 1999 to 2002 and Jeju from 2000 to 2002, respectively. “Jangbeol 101” showed semi-erect growth habit in fall and spring and medium type in length of flag leaf and upper internode. Plant height of “Jangbeol 101” was short compared to that of standard variety, “Ambassador” and heading date was delayed about 2 days as 14th May compared to Ambassador. Characters such as winter hardiness, regrowth, moisture tolerance, disease resistance of “Jangbeol 101” were stronger or better than those of Ambassador. “Jangbeol 101” showed 9% higher dry matter yield as 12,374 kg/ha compared to Amabassador. Nutritive value was appeared to be similar in both varieties.

A Study on the Efficient Compliance Method for Airworthiness Certification in the field of Flying Qualities of Military Aircraft (군용항공기 비행성 분야의 효율적인 감항인증 입증방법에 대한 고찰)

  • Kang, Myungsoo;Kim, Chong-sup;Koh, GiOk;Lim, Sang-soo;Kim, Byoung soo
    • Journal of Aerospace System Engineering
    • /
    • v.16 no.4
    • /
    • pp.95-108
    • /
    • 2022
  • Airworthiness certification is critical, in ensuring the flight safety of military aircraft for development tests and production operations. The MIL-HDBK-516C, latest airworthiness certification document, handles the field of flying qualities in Chapter 6 (flight technology), and refers to specific chapters of MIL-STD-1797B, which is the specification document for developing military aircraft. Since the MIL-STD-1797B released in 2006 by the U.S. Department of Defense is not disclosed to other countries, the Chapter 6 (flight technology) of MIL-HDBK-516B Expanded, the former certification standards pursuant to flying qualities, has to be applied to military aircraft being developed in the Republic of Korea. However the requirements of Chapter 6 of MIL-HDBK-516B Expanded comprise unclear sentences, because of contents from various development specifications. Also, clarification is needed in that the same requirements have to be verified in different criteria. In this paper, the results of this study present an effective verification method, for acquiring the airworthiness certification in field of flying qualities based on MIL-HDBK-516B Expanded.