以 QuEChERS为前处理方法,超高效液相色谱-串联质谱为检测仪器,建立了蔬菜中 250 种农药残留的快速筛查检测方法.采用含1%(v/v)乙酸的乙腈溶液提取样品,以无水硫酸镁(MgSO4)作为脱水剂,经 MgSO4、丙基乙二胺(PSA)、石墨化碳(GCB)、C18混合净化剂净化,Waters ACQUITYTM UPLC BEH C18柱(100 mm×2. 1 mm, 1. 7 μm)分离,超高效液相色谱-串联质谱进行测定.实验详细考察了 MgSO4、PSA、GCB、C18 用量对农药添加回收率的影响,结果表明,2 mL提取上清液中加入300 mg MgSO4、200 mg PSA、10 mg GCB和100 mg C18时净化效果最好.250种农药在韭菜中3个添加水平下的回收率为60. 1%~120. 0%,相对标准偏差( RSD)为 3. 5%~19. 5%;检出限为 0. 01~50. 00 μg/kg.该方法简便、快速、可靠,可用于蔬菜中多种农药残留的快速筛查与确证的日常工作中,具有一定的推广价值.
A multiresidue analytical method for the determination of 250 pesticide residues in vegetables was developed by using QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry ( UPLC-MS/MS ). The target compounds were extracted with acetonitrile containing 1%(v/v)acetic acid,purified by a mixed sorbent of MgSO4,primary secondary amine ( PSA),graphitized carbon black( GCB)and C18,separated on a Waters ACQUITY TM UPLC BEH C18 column(100 mm×2. 1 mm,1. 7 μm)and detected by UPLC-MS/MS. Anhydrous magnesium sulfate was used as a dewatering agent. The effects of the amounts of MgSO4,PSA,GCB and C18 added on the recoveries of 250 pesticides were investigated. The results showed that the purifica-tion effect was best when 300 mg MgSO4,200 mg PSA,10 mg GCB and 100 mg C18 in 2 mL of the extract were added. For the 250 pesticide residues,the limits of detection( LODs)of the method were from 0. 01 to 50. 00 μg/kg. The recoveries obtained ranged from 60. 1% to 120% at three spiked levels in Chinese chives with the relative standard deviations between 3. 5% and 19. 5%using matrix matched external standard method. The results showed that the method is able to meet requirements of the multiresidue detection of the 250 pesticides in vegetable. The method has the advantages of rapidity,simplicity,high sensitivity and better purification effect. It is suit-able for the rapid determination of the common pesticides in vegetables,and it provides a strong guarantee for the risk assessments of the quality and safety of vegetables.
参考文献
| [1] | Lesueur C.;Knittl P.;Gartner M.;Mentler A.;Fuerhacker M..Analysis of 140 pesticides from conventional farming foodstuff samples after extraction with the modified QuECheRS method.[J].Food Control,20089(9):906-914. |
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