农产品中多环芳烃的测定

IF 0.7 Q4 CHEMISTRY, ANALYTICAL Methods and Objects of Chemical Analysis Pub Date : 2021-01-01 DOI:10.17721/moca.2021.127-136
К.К. Tsymbaliuk, O. Snurnikova, K. Melnyk, E.M. Fadeev, V. Antonovich
{"title":"农产品中多环芳烃的测定","authors":"К.К. Tsymbaliuk, O. Snurnikova, K. Melnyk, E.M. Fadeev, V. Antonovich","doi":"10.17721/moca.2021.127-136","DOIUrl":null,"url":null,"abstract":"The procedure for the determination of polycyclic aromatic hydrocarbons (PAH) in agricultural products on the example of five crops (rapeseed, sunflower, flax, corn, soybeans) by gas chromatography mass spectrometry (GC-MS) was developed. It was showed the advantage of using binary mixtures of organic solvents \"hexanedichloromethane\" for PAH extraction. The time of Soxhlet extraction is from 6 to 8 hours at optimized conditions. The fractionation and purification of extracts by column chromatography on deactivated alumina was optimized. The article presents the optimization of sample injection in the programmed temperature vaporization (PTV) mode, parameters of gas chromatographic separation and mass spectrometric detection in determining 16 priority PAH in agricultural products. The recoveries, correctness and accuracy of the proposed method were checked by “spikes” with concentrations 0.5, 1.0, 2.5, 5.0 μg kg-1. The linearity of the method was determined by calibration curves obtained for three measurements of calibration solutions with concentrations of 0.5-100 ng mL-1. The effectiveness of the proposed combination of sample preparation and analysis by PTV-GC-MS was studied for linearity, accuracy, matrix effects and reproducibility. The method was validated by linearity, accuracy, matrix effect and reproducibility.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":"409 1","pages":""},"PeriodicalIF":0.7000,"publicationDate":"2021-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Determination of Polycyclic Aromatic Hydrocarbons in Agricultural Products\",\"authors\":\"К.К. Tsymbaliuk, O. Snurnikova, K. Melnyk, E.M. Fadeev, V. Antonovich\",\"doi\":\"10.17721/moca.2021.127-136\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"The procedure for the determination of polycyclic aromatic hydrocarbons (PAH) in agricultural products on the example of five crops (rapeseed, sunflower, flax, corn, soybeans) by gas chromatography mass spectrometry (GC-MS) was developed. It was showed the advantage of using binary mixtures of organic solvents \\\"hexanedichloromethane\\\" for PAH extraction. The time of Soxhlet extraction is from 6 to 8 hours at optimized conditions. The fractionation and purification of extracts by column chromatography on deactivated alumina was optimized. The article presents the optimization of sample injection in the programmed temperature vaporization (PTV) mode, parameters of gas chromatographic separation and mass spectrometric detection in determining 16 priority PAH in agricultural products. The recoveries, correctness and accuracy of the proposed method were checked by “spikes” with concentrations 0.5, 1.0, 2.5, 5.0 μg kg-1. The linearity of the method was determined by calibration curves obtained for three measurements of calibration solutions with concentrations of 0.5-100 ng mL-1. The effectiveness of the proposed combination of sample preparation and analysis by PTV-GC-MS was studied for linearity, accuracy, matrix effects and reproducibility. The method was validated by linearity, accuracy, matrix effect and reproducibility.\",\"PeriodicalId\":18626,\"journal\":{\"name\":\"Methods and Objects of Chemical Analysis\",\"volume\":\"409 1\",\"pages\":\"\"},\"PeriodicalIF\":0.7000,\"publicationDate\":\"2021-01-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Methods and Objects of Chemical Analysis\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.17721/moca.2021.127-136\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q4\",\"JCRName\":\"CHEMISTRY, ANALYTICAL\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Methods and Objects of Chemical Analysis","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.17721/moca.2021.127-136","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"CHEMISTRY, ANALYTICAL","Score":null,"Total":0}
引用次数: 0

摘要

以油菜籽、向日葵、亚麻、玉米、大豆等5种农作物为例,建立了气相色谱-质谱法测定农产品中多环芳烃(PAH)的方法。结果表明,采用二元混合有机溶剂“己二氯甲烷”萃取多环芳烃具有优势。在优化条件下,索氏提取时间为6 ~ 8小时。优化了失活氧化铝柱层析法分离纯化提取物的工艺条件。本文介绍了程序温度汽化(PTV)进样方式的优化、气相色谱分离和质谱检测参数在测定农产品中16种重点多环芳烃中的应用。采用浓度分别为0.5、1.0、2.5、5.0 μg kg-1的“峰值”检测方法的回收率、正确性和准确性。通过对浓度为0.5 ~ 100 ng mL-1的校准溶液进行三次测量得到的校准曲线来确定该方法的线性度。研究了PTV-GC-MS样品制备与分析相结合的线性、准确性、基质效应和重现性。通过线性度、准确度、基质效应和重现性验证了该方法的有效性。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
查看原文
分享 分享
微信好友 朋友圈 QQ好友 复制链接
本刊更多论文
Determination of Polycyclic Aromatic Hydrocarbons in Agricultural Products
The procedure for the determination of polycyclic aromatic hydrocarbons (PAH) in agricultural products on the example of five crops (rapeseed, sunflower, flax, corn, soybeans) by gas chromatography mass spectrometry (GC-MS) was developed. It was showed the advantage of using binary mixtures of organic solvents "hexanedichloromethane" for PAH extraction. The time of Soxhlet extraction is from 6 to 8 hours at optimized conditions. The fractionation and purification of extracts by column chromatography on deactivated alumina was optimized. The article presents the optimization of sample injection in the programmed temperature vaporization (PTV) mode, parameters of gas chromatographic separation and mass spectrometric detection in determining 16 priority PAH in agricultural products. The recoveries, correctness and accuracy of the proposed method were checked by “spikes” with concentrations 0.5, 1.0, 2.5, 5.0 μg kg-1. The linearity of the method was determined by calibration curves obtained for three measurements of calibration solutions with concentrations of 0.5-100 ng mL-1. The effectiveness of the proposed combination of sample preparation and analysis by PTV-GC-MS was studied for linearity, accuracy, matrix effects and reproducibility. The method was validated by linearity, accuracy, matrix effect and reproducibility.
求助全文
通过发布文献求助,成功后即可免费获取论文全文。 去求助
来源期刊
CiteScore
1.00
自引率
14.30%
发文量
12
期刊介绍: The journal "Methods and objects of chemical analysis" is peer-review journal and publishes original articles of theoretical and experimental analysis on topical issues and bio-analytical chemistry, chemical and pharmaceutical analysis, as well as chemical metrology. Submitted works shall cover the results of completed studies and shall make scientific contributions to the relevant area of expertise. The journal publishes review articles, research articles and articles related to latest developments of analytical instrumentations.
期刊最新文献
Systematic Review and Guidelines for Management of Scrotal Inguinal Hernias. Study of the Biochemical Potential of Wild Fruit of the Caucasus Medar (Mespilus caucasics L.) in the Post-Harvest Period Chromatographic Determination of the Chemical Composition of Apple Chips Extract Development, Optimization, and Validation of a Novel HPLC Method for Simultaneous Quantification of Artesunate and Amodiaquine in Tablet Formulations Analytical Validation of a Reversed-Phase Ion Pairing HPLC-DAD Method for the Simultaneous Determination of Anthropogenic Pollutants
×
引用
GB/T 7714-2015
复制
MLA
复制
APA
复制
导出至
BibTeX EndNote RefMan NoteFirst NoteExpress
×
×
提示
您的信息不完整,为了账户安全,请先补充。
现在去补充
×
提示
您因"违规操作"
具体请查看互助需知
我知道了
×
提示
现在去查看 取消
×
提示
确定
0
微信
客服QQ
Book学术公众号 扫码关注我们
反馈
×
意见反馈
请填写您的意见或建议
请填写您的手机或邮箱
已复制链接
已复制链接
快去分享给好友吧!
我知道了
×
扫码分享
扫码分享
Book学术官方微信
Book学术文献互助
Book学术文献互助群
群 号:481959085
Book学术
文献互助 智能选刊 最新文献 互助须知 联系我们:info@booksci.cn
Book学术提供免费学术资源搜索服务,方便国内外学者检索中英文文献。致力于提供最便捷和优质的服务体验。
Copyright © 2023 Book学术 All rights reserved.
ghs 京公网安备 11010802042870号 京ICP备2023020795号-1