液相色谱-串联质谱法测定氟噻草胺在小麦上的残留行为及其膳食风险评估

Determination of Residual Behavior of Flufenacet in Wheat and its Dietary Risk Assessment by Liquid Chromatography-Tandem Mass Spectrometry

  • 摘要: 本研究建立了液相色谱-串联质谱法测定小麦中氟噻草胺及其代谢物残留。结果表明,氟噻草胺及其代谢物在0.001~0.5 mg/L浓度范围内的线性关系良好,相关系数大于0.999;在3种不同浓度的回收实验中,氟噻草胺及其代谢物在小麦中的添加回收率为70.7%~119.4%,相对标准偏差为0.5%~5.9%,氟噻草胺和氟噻草胺巯基乙酸亚砜、氟噻草胺OA和氟噻草胺ESA的方法定量限分别为0.01、0.05 mg/kg。采用该方法测定10个地区采收期的小麦样品,麦粒和秸秆中氟噻草胺和氟噻草胺巯基乙酸亚砜残留量均小于0.010 mg/kg,氟噻草胺OA残留量介于0.050~0.38 mg/kg之间,氟噻草胺ESA残留量小于0.050 mg/kg,氟噻草胺(总)残留量介于0.12~0.69 mg/kg之间。膳食风险评估结果表明,普通人群氟噻草胺的国家估算每日摄入量(NEDI)为0.02687 mg,氟噻草胺的风险熵为8.5%,表明小麦中氟噻草胺残留对一般人群健康不会产生不可接受的风险。

     

    Abstract: A method of liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the determination of flufenacet and its metabolites in wheat. The results showed that the linear relationship of flufenacet and its metabolites is good in the concentration of 0.001-0.5 mg/L, and the correlation coefficient is greater than 0.999. In three different concentration levels, the recoveries of flufenacet, flufenacet thioglycolate sulfoxide, flufenacet OA and flufenacet ESA in wheat are 89.1%-119.4%, 70.7%-113.0%, 72.0%-105.3%, 74.1%-114.8% with the relative standard deviations (RSDs) range of 0.5%-3.1%, 2.2%-5.6%, 1.6%-3.4%, 1.4%-5.9%, respectively. The limits of quantitation (LOQs) of flufenacet and flufenacet thioglycolate sulfoxide, flufenacet OA and flufenacet ESA are 0.01, 0.05 mg/kg, respectively. The method was used to determine the wheat samples in ten areas. During the harvesting, the residues of flufenacet and flufenacet thioglycolate sulfoxide in wheat grains and stalks period are all less than 0.010 mg/kg, flufenacet OA are 0.050-0.38 mg/kg, flufenacet ESA are less than 0.050 mg/kg, and the total residues of flufenacet are less than 0.12-0.69 mg/kg. Dietary risk assessment was calculated according to the dietary risk assessment model. The results showed that the daily intake (NEDI) of flufenacet in winter wheat for general population is 0.02687 mg, and the risk entropy of flufenacet is 8.5%, indicating that the dose of flufenacet in wheat does not pose an unacceptable risk to the health of the general population. There are some uncertainties in risk assessment, which are mainly reflected in three aspects: 1) No chlorine-related information has been collected from the database of the FAO/WHO Joint Meeting on Pesticide Residues, and no reference dose has been found, so acute dietary intake risk assessment cannot be carried out. 2) The maximum residue limit of registered crops in various countries was used for the residual data of flufenacet, and the median residue value could not be obtained, and the processing factor of cooking process was not considered, so the calculated risk entropy was high. 3) In this paper, only wheat was used as a single exposure route to exposure, while daily residents were also exposed to flufenacet through other foods, so there are still some limitations in the overall risk assessment of flufenacet exposure for residents.

     

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