植物保护
植物保護
식물보호
PLANT PROTECTION
2014年
6期
112-115,130
,共5页
李广领%郭梅燕%谷珊山%董丽红%刘博%郭文举%陈锡岭
李廣領%郭梅燕%穀珊山%董麗紅%劉博%郭文舉%陳錫嶺
리엄령%곽매연%곡산산%동려홍%류박%곽문거%진석령
氟磺胺草醚%花生植株%花生籽粒%花生田土壤%基质分散萃取%残留分析
氟磺胺草醚%花生植株%花生籽粒%花生田土壤%基質分散萃取%殘留分析
불광알초미%화생식주%화생자립%화생전토양%기질분산췌취%잔류분석
fomesafen%peanut plant%peanut%peanut field soil%dispersive solid phase extraction%residues analysis
在前人研究基础上,确立了花生植株以甲醇、乙二胺-N-丙基硅烷(PSA)和石墨化炭黑(GCB)为基质分散萃取材料,花生籽粒和田间土壤分别以酸化甲醇和乙腈为分散萃取溶剂,以PSA为基质净化材料的3类氟磺胺草醚残留样品前处理程序,建立并优化了花生籽粒、花生植株和田间土壤氟磺胺草醚残留高效液相色谱检测方法。结果显示,氟磺胺草醚在0.05~10.0 mg/L质量浓度范围内与对应色谱峰积分面积线性响应良好,回归方程为y=2.5628 x-0.0068(r2=0.9998)。在0.05~0.5 mg/kg氟磺胺草醚添加范围内,花生籽粒、植株和田间土壤中的平均回收率为85.6%~113.5%,相对标准偏差为1.5%~9.7%。花生植株、籽粒和田间土壤中氟磺胺草醚的检出限分别为0.024、0.029和0.031 mg/kg。基质效应试验结果表明,该样品前处理方法获得的分析样品基质效应不明显,表明该残留样本前处理方法和样品检测方法简便、高效、经济、可靠,可满足氟磺胺草醚在花生植株、籽粒及田间土壤中残留的定量检测要求。
在前人研究基礎上,確立瞭花生植株以甲醇、乙二胺-N-丙基硅烷(PSA)和石墨化炭黑(GCB)為基質分散萃取材料,花生籽粒和田間土壤分彆以痠化甲醇和乙腈為分散萃取溶劑,以PSA為基質淨化材料的3類氟磺胺草醚殘留樣品前處理程序,建立併優化瞭花生籽粒、花生植株和田間土壤氟磺胺草醚殘留高效液相色譜檢測方法。結果顯示,氟磺胺草醚在0.05~10.0 mg/L質量濃度範圍內與對應色譜峰積分麵積線性響應良好,迴歸方程為y=2.5628 x-0.0068(r2=0.9998)。在0.05~0.5 mg/kg氟磺胺草醚添加範圍內,花生籽粒、植株和田間土壤中的平均迴收率為85.6%~113.5%,相對標準偏差為1.5%~9.7%。花生植株、籽粒和田間土壤中氟磺胺草醚的檢齣限分彆為0.024、0.029和0.031 mg/kg。基質效應試驗結果錶明,該樣品前處理方法穫得的分析樣品基質效應不明顯,錶明該殘留樣本前處理方法和樣品檢測方法簡便、高效、經濟、可靠,可滿足氟磺胺草醚在花生植株、籽粒及田間土壤中殘留的定量檢測要求。
재전인연구기출상,학립료화생식주이갑순、을이알-N-병기규완(PSA)화석묵화탄흑(GCB)위기질분산췌취재료,화생자립화전간토양분별이산화갑순화을정위분산췌취용제,이PSA위기질정화재료적3류불광알초미잔류양품전처리정서,건립병우화료화생자립、화생식주화전간토양불광알초미잔류고효액상색보검측방법。결과현시,불광알초미재0.05~10.0 mg/L질량농도범위내여대응색보봉적분면적선성향응량호,회귀방정위y=2.5628 x-0.0068(r2=0.9998)。재0.05~0.5 mg/kg불광알초미첨가범위내,화생자립、식주화전간토양중적평균회수솔위85.6%~113.5%,상대표준편차위1.5%~9.7%。화생식주、자립화전간토양중불광알초미적검출한분별위0.024、0.029화0.031 mg/kg。기질효응시험결과표명,해양품전처리방법획득적분석양품기질효응불명현,표명해잔류양본전처리방법화양품검측방법간편、고효、경제、가고,가만족불광알초미재화생식주、자립급전간토양중잔류적정량검측요구。
A method has been developed for determining fomesafen residues in peanut plants,peanuts and peanut field soil by high performance liquid chromatography(HPLC). Fomesafen residues in peanut plants was extracted by methanol and then purified by primary secondary amine(PSA)and graphitized carbon black(GCB),and fome-safen residues in peanuts or soil was extracted by methanol or acetonitrile(containing 1% formic acid),and then purified by PSA.Then these detection samples were detected by HPLC under the optimal conditions. The results showed,under the optimal conditions,the calibration curves showed good linearity(y= 2.562 8 x-0.006 8,r2=0.999 8)at 0.05 10.0 mg/L concentration of fomesafen,the average recoveries of fomesafen in peanut plants, peanuts,peanut field soil at the three spiked concentration levels ranged from 85.6% to 113.5% ,and the relative standard deviations was 1 .5% 9 .7% . The lowest concentration detected of fomesafen in peanut plants,peanuts and peanut field soil were 0.024 mg/kg,0.029 mg/kg and 0.031 mg/kg,respectively. The matrix effect of the method was studied and there was no significant difference. In sum,the method was simple,efficient,economy and reliable,which can meet quantitative detection requirements in peanut,peanut plants and soil.