Navickiene Sandro, Santos Luis Fabrício Santana, Dos Reis Silva Alexandre
Universidade Federal de Sergipe, Departament de Química, Av. Marechal Rondon s/nº, São Cristóvão SE 49100-000, Brazil.
J AOAC Int. 2019 Mar 1;102(2):619-624. doi: 10.5740/jaoacint.18-0172. Epub 2018 Oct 5.
Pesticides are applied for pest control during the production of cereal grains used in beer production. Given the risks for consumers, it is important to analyze the pesticide residues. Quick, easy, cheap, effective, rugged, and safe (QuEChERS)-based methods are very effective, and improvement in the cleanup step is an important approach. Primary secondary amine (PSA) and magnesium silicate were evaluated for dispersive-solid-phase extraction (d-SPE) cleanup step in extracts provided by the QuEChERS method in combination with GC-tandem MS for the determination of acetamiprid, terburfos, alachlor, ametryn, atrazine, azoxystrobin, carbofuran, carbosulfan, cypermethrin, deltamethrin, difenoconazole, esfenvalerate, flutriafol, thiamethoxam, and parathion-methyl in lager beer. The amount of 50 mg of magnesium silicate was suitable for cleaning up beer extract as an alternative d-SPE material to PSA. The method was validated using beer fortified with pesticides at three concentration levels (0.002, 0.01, and 0.1 μg/mL). Average recoveries ranged from 70 to 123%, with RSDs between 0.3 and 10.5 %. Matrix effects were observed by comparing the slope of matrix-matched standard calibration with that of solvent. The method provided good linearity at the concentration levels of 0.001-2.5 μg/mL. Detection limits ranged from 0.0001 to 0.0007 μg/mL and quantification limits ranged from 0.001 to 0.006 μg/mL. The method was applied to nine beer brands. Results showed that magnesium silicate is an efficient alternative cleanup material to reduce analysis costs while maintaining the method reliability and accuracy. Magnesium silicate was effective as adsorbent for d-SPE step in the analysis of pesticides in beer.
在用于啤酒生产的谷物生产过程中会使用农药来控制害虫。鉴于对消费者存在风险，分析农药残留很重要。基于快速、简便、廉价、有效、耐用和安全（QuEChERS）的方法非常有效，而改进净化步骤是一种重要途径。在QuEChERS方法结合气相色谱 - 串联质谱法测定贮藏啤酒中啶虫脒、特丁硫磷、甲草胺、莠灭净、阿特拉津、嘧菌酯、克百威、丁硫克百威、氯氰菊酯、溴氰菊酯、苯醚甲环唑、乙氰菊酯、氟环唑、噻虫嗪和甲基对硫磷的提取物中，评估了伯仲胺（PSA）和硅酸镁用于分散固相萃取（d - SPE）净化步骤的效果。50毫克硅酸镁的量适合作为替代PSA的d - SPE材料来净化啤酒提取物。该方法在添加了三种浓度水平（0.002、0.01和0.1μg/mL）农药的啤酒中进行了验证。平均回收率在70%至123%之间，相对标准偏差在0.3%至10.5%之间。通过比较基质匹配标准校准曲线与溶剂校准曲线的斜率来观察基质效应。该方法在0.001 - 2.5μg/mL的浓度水平下具有良好的线性。检测限在0.0001至0.0007μg/mL之间，定量限在0.001至0.006μg/mL之间。该方法应用于九个啤酒品牌。结果表明，硅酸镁是一种有效的替代净化材料，可在保持方法可靠性和准确性的同时降低分析成本。在啤酒中农药分析的d - SPE步骤中，硅酸镁作为吸附剂是有效的。
