生境中醌类衍生物的分析控制问题

M. S. Grechina, Alena V. Suslova, Viktoriya V. Belitskaya
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摘要

介绍。从环境物和进口食品安全的规范性和方法学保证的角度出发,对空气和柑橘类水果中醌类杀菌剂二硫菊酮的分析方法进行了优化。材料和方法。采用多反应监测(MRM)模式,以静电喷雾为电离源,采用三重四极杆质量检测器(HPLC-MS/MS)串联液相质谱法进行测量。将空气中的物质浓缩在基于多孔聚合物吸附剂的Tenax TA吸附管中,然后用丙酮从管中提取二硫菊酮。在硫酸镁盐、氯化钠盐、二代和三代柠檬酸钠盐存在下,提取酸化乙腈(选择最佳pH为2),离心,并通过一次性注射器膜过滤器(QuEChERS技术)过滤,制备柑橘类水果样品。结果。所开发的技术在农业实践中对实际样品进行了试验。所显示的二硫磷水平不超过定量测定的下限:环境空气中的0.000071 mg/m3 (RISL值为0.0001 mg/m3)和柑橘类水果中的0.01 mg/kg (MRL值为3 mg/kg)。结论。所开发的方法已被批准为官方文件,并补充了大气空气和进口食品控制分析方法的基础。
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On the issue of analytical control of quinone derivatives in habitats
Introduction. In the direction of normative and methodological assurance of the safety of environmental objects and imported food products, analytical approaches to the determination of a fungicide of the quinone class - dithianone in the air and citrus fruits were optimized. Materials and methods. Measurements were performed by tandem liquid mass spectrometry with a triple quadrupole mass detector (HPLC-MS/MS) in multiple reaction monitoring (MRM) mode using electrostatic spray as the ionization source. The substance from the air was concentrated on Tenax TA sorption tubes based on a porous polymer sorbent, followed by extraction of dithianone from the tubes with acetone. The preparation of samples of citrus fruits was carried out by extraction of acidified acetonitrile (selected optimal pH 2) in the presence of salts of magnesium sulfate, sodium chloride and sodium citrate two- and three-substituted, followed by centrifugation and filtration of the extract through disposable syringe membrane filters (QuEChERS technology). Results. The developed techniques were tested on real samples using the pesticide in agricultural practice. The revealed levels of dithianon do not exceed the lower limit of quantitative determination: 0.000071 mg/m3 in ambient air (with an RISL value of 0.0001 mg/m3) and 0.01 mg/kg in citrus fruits (with an established MRL value of 3 mg/kg). Conclusion. The developed methods are approved as official documents and supplement the base of analytical methods in terms of control of atmospheric air and imported food products.
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