К.К. Tsymbaliuk, O. Snurnikova, K. Melnyk, E.M. Fadeev, V. Antonovich
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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。
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.
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.