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首页> 外文期刊>Journal of AOAC International >Optimization of detection conditions and single-laboratory validation of a multiresidue method for the determination of 135 pesticides and 25 organic pollutants in grapes and wine by gas chromatography time-of-flight mass spectrometry.
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Optimization of detection conditions and single-laboratory validation of a multiresidue method for the determination of 135 pesticides and 25 organic pollutants in grapes and wine by gas chromatography time-of-flight mass spectrometry.

机译：气相色谱飞行时间质谱法测定葡萄和葡萄酒中135种农药和25种有机污染物的检测条件的优化和多实验室方法的单实验室验证。

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摘要

Single-laboratory validation of a multiresidue method was conducted for the determination of 135 pesticides, 12 dioxin-like polychlorinated biphenyls, 12 polyaromatic hydrocarbons and bisphenol A in grapes and wine by GC/time-of-flight MS in a total run time of 48 min. The method is based on extraction with ethyl acetate in a sample-to-solvent ratio of 1:1, followed by selective dispersive SPE cleanup for grapes and wine. The GC-MS conditions were optimized for the chromatographic separation and to achieve highest S/N for all 160 target analytes, including temperature-sensitive compounds, such as captan and captafol, that are prone to degradation during analysis. An average recovery of 80-120% with relative s.d. <10% could be attained for all analytes except 17, for which the average recoveries were 70-80%. LOQ ranged within 10-50 ng/g, with <25% expanded uncertainties, for 155 compounds in grapes and 151 in wine. In the incurred grape and wine samples, residues of buprofezin, chlorpyriphos, metalaxyl and myclobutanil were detected, with a relative s.d. of <5% (n = 6); the results were statistically similar to those obtained in previously reported and validated methods.
机译：采用气相色谱/飞行时间质谱仪进行多实验室方法的单实验室验证，用于测定葡萄和葡萄酒中的135种农药，12种二恶英样多氯联苯，12种多芳烃和双酚A，总运行时间为48分钟该方法基于样品与溶剂之比为1：1的乙酸乙酯萃取，然后对葡萄和葡萄酒进行选择性分散SPE净化。 GC-MS条件已针对色谱分离进行了优化，并针对所有160种目标分析物（包括对温度敏感的化合物，如captan和captafol）在分析过程中易于降解，实现了最高的信噪比。相对标准偏差的平均回收率为80-120％。对于除17种以外的所有分析物，其平均回收率为70-80％，均可以达到<10％。对于葡萄中的155种化合物和葡萄酒中的151种化合物，LOQ的范围在10-50 ng / g之间，不确定度<25％。在产生的葡萄和葡萄酒样品中，检测到了丁苯丙酸，毒死pho，甲霜灵和霉菌丁的残留，其相对标准偏差为s。 <5％（ n = 6）;结果在统计学上与以前报道和验证的方法相似。

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