Mereke Alimzhanova, Yerkanat Syrgabek, Pedro Antonio Garcia Encina
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引用次数: 0
Abstract
A simple and environmentally friendly method based on miniaturized headspace solid-phase microextraction (Mini-HS-SPME) coupled with gas chromatography–mass spectrometry (GC-MS) was developed for the identification and quantification of ten pesticides (atrazine, simazine, prometryn, metribuzin, cyanazine, fluroxypyr-meptyl, tebuconazole, epoxiconazole, quizalofop-methyl, and boscalid) in grape samples. Key extraction parameters were optimized, including extraction temperature, extraction time, selection of the optimal fiber, incubation time, effect of salt, volume of sample, and pH. Final extraction conditions included the use of 200 µL of sample using PDMS 100 µm fiber in headspace mode at 90°C for 30 min. The Mini-HS-SPME coupled with the GC-MS method has been successfully validated in terms of linearity, recovery, and accuracy. The studied linear range of pesticides was 5–1000 ng mL−1. The limit of detection and limit of quantification ranged between 0.09–3.0 ng mL⁻¹ and 0.2–10.1 ng mL⁻¹, respectively. In conclusion, this research presents a method for detecting pesticides in terms of miniaturization, and evaluation of environmental friendliness and applicability using modern GAPI, AGREEprep, and BAGI tools.
建立了小型顶空固相微萃取(Mini-HS-SPME) -气相色谱-质谱联用技术对葡萄样品中10种农药(阿特拉津、西马辛、prometryn、metriz嗪、cyanazine、氟氧苄啶-甲基、tebuconazole、epoxiconazole、quizalofopop甲基和boscalid)进行鉴定和定量的方法。优化提取关键参数,包括提取温度、提取时间、最佳纤维的选择、培养时间、盐的影响、样品体积和ph。最终提取条件为:使用200µL样品,使用PDMS 100µm纤维,在顶空模式下,在90°C下,提取30 min。Mini-HS-SPME结合GC-MS方法在线性、回收率和准确性方面都得到了成功验证。杀虫剂的线性范围为5 ~ 1000 ng mL−1。检测限和定量限分别在0.09-3.0 ng mL⁻¹和0.2-10.1 ng mL⁻¹之间。综上所述,本研究提出了一种基于现代GAPI、AGREEprep和BAGI工具的农药小型化检测、环境友好性和适用性评价方法。
期刊介绍:
The Journal of Separation Science (JSS) is the most comprehensive source in separation science, since it covers all areas of chromatographic and electrophoretic separation methods in theory and practice, both in the analytical and in the preparative mode, solid phase extraction, sample preparation, and related techniques. Manuscripts on methodological or instrumental developments, including detection aspects, in particular mass spectrometry, as well as on innovative applications will also be published. Manuscripts on hyphenation, automation, and miniaturization are particularly welcome. Pre- and post-separation facets of a total analysis may be covered as well as the underlying logic of the development or application of a method.