二氯喹啉酸及其代谢物和莠去津在高粱中的残留检测及膳食风险评估

Determination and dietary risk assessment of quinclorac and atrazine residues in sorghum

[目的]采用超高效液相色谱串联质谱检测高粱中二氯喹啉酸及其代谢物二氯喹啉酸甲酯和莠去津残留量,并对其膳食摄入风险进行了评估。[方法]样品经1%乙酸乙腈作提取,经GCB净化,外标法定量,超高效液相色谱串联质谱检测。[结果]高粱基质中的二氯喹啉酸及其代谢物和莠去津在0.005~1.0 mg/L范围内呈良好线性(R2=0.99);在0.01~2.0 mg/kg加标水平范围内高粱基质中的二氯喹啉酸平均回收率为83%~90%,RSD为7.04%~9.62%;二氯喹啉酸甲酯的平均回收率为83%~103%,RSD%为1.32%~8.73%;莠去津的平均回收率为83%~104%,RSD为1.91%~9.84%,3种农药的定量限(LOQ)均为0.01 mg/kg。膳食风险评估结果表明:成年男女二氯喹啉酸的国家估算每日摄入量分别为7.3、8.9μg/kg b.w.·d,占日允许摄入量的1.82%、2.22%;成年男女二氯喹啉酸的国家估算短期摄入量分别为84、103μg/kg b.w.·d,占急性参考剂量的4.22%、5.13%。[结论]该方法操作简便,适用于高粱中二氯喹啉酸及其代谢物和莠去津残留的检测。高粱收获期采收安全,认为对一般人群不会产生不可接受的膳食摄入风险。

[Aims] This study aims to determinate the residue of quinclorac and its metabolite and atrazine in sorghum by UPLC-MS/MS, and to evaluate the dietary risk. [Methods] The samples were extracted with acetonitrile containing1% acetic acid and detected by UPLC-MS/MS after being cleaned up by GCB powder. The external standard method was used to quantify. [Results] The results showed that the linearities of quinclorac and its metabolite and atrazine in sorghum were good at spiked levels from 0.005-1.0 mg/L. At addition levels of 0.01-2.0 mg/kg, the average recoveries of quinclorac in sorghum were in the range of 83%-90% with relative deviations of 7.04%-9.62%, while the average recoveries and relative deviations of quinclorac-methyl ester were 83%-103% and 1.32%-8.73%, and of atrazine were83%-104% and 1.91%-9.84%. The limit of quantification(LOQ) was 0.01 mg/kg. Through the dietary risk analysis, it can be concluded that the national estimated daily intake(NEDI) of the general male and female population in quinclorac is 7.3 and 8.9 μg/kg b.w.·d, accounting for about 1.82% and 2.22% of the allowable daily intake. The national estimated short term intake(NESTI) of the general male and female population in quinclorac is 84 and103 μg/kg b.w.·d, accounting for about 4.22% and 5.13% of the acute reference dose. [Conclusions] The method shows the advantages of simplicity and rapidness, which can be used in residue analysis of quinclorac and its metabolite and atrazine in sorghum. It shows the safety of sorghum during harvest period, it will not pose unacceptable risks to the health of the general population.