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Determination of Pesticide Residues in Fruit-Based Soft Drinks

机译:水果软饮料中农药残留的测定

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Here we report the first worldwide reconnaissance study of the presence and occurrence of pesticides in fruit-based soft drinks. While there are strict regulations and exhaustive controls for pesticides in fruits, vegetables, and drinking water, scarce attention has been paid to highly consumed derivate products, which may contain these commodities as ingredients. In the case of the fruit-based soft drinks industry, there are no clear regulations, relating to pesticides, which address them, even when there is significant consumption in vulnerable groups such as children. In this work, we have developed a screening method to search automatically for up to 100 pesticides in fruit-based soft drinks extracts based on the application of liquid chromatography-electrospray time-of-flight mass spectrometry (LC-TOF MS). The sample extracts injected were obtained by a preliminary sample treatment step based on solid-phase extraction using hydrophilic-lipophilic balanced polymer-based reverse phase cartridges and methanol as eluting solvent. Subsequent identification, confirmation, and quantitation were carried out by LC-TOF MS analysis: the confirmation of the target species was based on retention time matching and accurate mass measurements of protonated molecules ([M + H]~(+)) and fragment ions (obtaining accuracy errors typically lower than 2 ppm). With the proposed method, we measured over 100 fruit-based soft drink samples, purchased from 15 different countries from companies with brands distributed worldwide and found relatively large concentration levels of pesticides in most of the samples analyzed. The concentration levels detected were of the micrograms per liter level, low when considering the European maximum residue levels (MRLs) set for fruits but very high (i.e., 300 times) when considering the MRLs for drinking or bottled water. The detected pesticides (carbendazim, thiabendazole, imazalil and its main degradate, prochloraz and its main degradate, malathion, and iprodione) are mainly those applied to crops in the final stages of production (postharvest treatment), some of them contain chlorine atoms in their structures. Therefore, steps should be taken with the aim of removing any traces of pesticides in these products, in order to avoid this source of pesticide exposure on the consumer, particularly on vulnerable groups with higher exposure, such as children.
机译:在这里,我们报告了第一个关于水果类软饮料中农药存在与否的全球侦查研究。尽管对水果,蔬菜和饮用水中的农药有严格的规定和详尽的控制措施,但很少注意高度消耗的衍生产品,这些产品可能含有这些商品。就水果类软饮料行业而言,即使在儿童等弱势群体中有大量消费,也没有针对农药的明确法规来解决这些问题。在这项工作中,我们开发了一种筛选方法,该方法基于液相色谱-电喷雾飞行时间质谱(LC-TOF MS)的应用,可以自动在基于水果的软饮料提取物中搜索多达100种农药。注入的样品提取物是通过基于固相萃取的初步样品处理步骤而获得的,该步骤使用亲水-亲脂平衡聚合物基反相色谱柱和甲醇作为洗脱溶剂进行固相萃取。随后的鉴定,确认和定量通过LC-TOF MS分析进行:目标物种的确认基于保留时间匹配和质子化分子([M + H]〜(+))和碎​​片离子的准确质量测量(获得的精度误差通常低于2 ppm)。通过提出的方法,我们测量了100多种基于水果的软饮料样品,这些样品是从15个不同的国家/地区购买的,这些公司的品牌分布于世界各地,并且在大多数被分析的样品中发现农药浓度相对较高。检测到的浓度水平为每升微克水平,考虑到为水果设定的欧洲最大残留水平(MRL)时较低,但考虑到饮用或瓶装水的最大残留限量时则很高(即300倍)。检出的农药(多菌灵,噻菌灵,咪唑和其主要降解物,丙草胺及其主要降解物,马拉硫磷和异丙嗪酮)主要是在生产的最后阶段(收获后处理)施用于作物的农药,其中一些农药中含有氯原子结构。因此,应采取措施消除这些产品中的任何农药残留,以避免这种农药对消费者的暴露,特别是对儿童等暴露率较高的弱势群体。

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