棉籽中环丙酰草胺及其代谢物残留检测及膳食摄入评估

Determination of Cyclanilide and Its Metabolite in Cottonseed and Risk Assessment for Dietary Residue Intake

[目的]建立环丙酰草胺及其代谢物在棉籽中的残留检测方法,并对棉籽中的残留量进行膳食摄入评估。[方法]样品中环丙酰草胺加乙腈提取、离心,上清液过滤膜后经超高效液相色谱三重四极杆串联质谱检测,外标法定量;样品中2,4-二氯苯胺加乙腈涡旋提取、离心,上清液经GCB和PSA净化,过滤膜后气相色谱电子捕获检测器检测,外标法定量。[结果]棉籽中环丙酰草胺和2,4-二氯苯胺平均回收率分别为80%~84%和75%~92%,相对标准偏差分别为0.56%~8.6%和4.4%~7.4%。棉籽中环丙酰草胺和2,4-二氯苯胺的最低检测浓度均为0.1 mg/kg。[结论]按试验设计进行施药,环丙酰草胺的普通人群国家估计每日摄入量占日允许摄入量的1.38%左右,认为对一般人群健康不会产生不可接受的风险。

[Aims]This study aims to establish an analytical method for the residues of cyclanilide and its metabolites in cotton,and to assess dietary intake risk of the residues in cotton seeds.[Methods]The residue cyclanilide was extracted with acetonitrile,centrifugated,the supernatant was filtered through the membranes,followed by analysis with high performance liquid chromatography-tandem mass spectrometry(LC-MS/MS).The residue 2,4-dichloroaniline was extracted with acetonitrile,centrifugated,and the supernatant was then purified via GCB and PSA.Then,2,4-dichloroaniline was analyzed with gas chromatography-electron capture detection(GC-ECD).[Results]The average recoveries of cyclanilide and 2,4-dichloroaniline in cotton seeds was from 80 to 84%and 75 to 92%,respectively,with relative standard deviations(RSD)ranging from 0.56 to 8.6%and 4.4 to 7.4%,respectively.The limits of quantification(LOQ)of cyclanilide and 2,4-dichloroaniline in cotton were both 0.1 mg/kg.[Conclusions]The result showed that the cyclanilide residues content only accounts for 1.38%of ADI when cotton was sprayed following the instruction of this design,and there was generally no unacceptable health risk as regarded.