浙江农业学报
浙江農業學報
절강농업학보
ACTA AGRICULTURAE ZHEJIANGENSIS
2014年
1期
131-134
,共4页
刘景坤%武春媛%邓晓%陈珊珊%李勤奋
劉景坤%武春媛%鄧曉%陳珊珊%李勤奮
류경곤%무춘원%산효%진산산%리근강
吡虫啉%啶虫脒%固相萃取-高效液相色谱法%定量限%回收率
吡蟲啉%啶蟲脒%固相萃取-高效液相色譜法%定量限%迴收率
필충람%정충미%고상췌취-고효액상색보법%정량한%회수솔
imidacloprid%acetamiprid%SPE-HPLC%LOQ%recovery
经过紫外扫描确定吡虫啉和啶虫脒的最大紫外吸收波长分别为270和246 nm,通过改变其比例优化出峰时间和分离度,确定V(乙腈)∶V(水)=3∶7为流动相,建立了两种农药的标准曲线,结果表明在0.05~5μg· mL-1范围内线性关系均良好。进行样品加标回收实验,用乙腈提取,C18固相萃取柱净化,上述条件进行下分析,0.1,0.5,1.5 mg· kg-1三个加标浓度回收率均在75%~110%,变异系数<5%,准确性和稳定性都较好,方法最低定量限0.01μg· g-1,完全可以用于实际样品的检测。
經過紫外掃描確定吡蟲啉和啶蟲脒的最大紫外吸收波長分彆為270和246 nm,通過改變其比例優化齣峰時間和分離度,確定V(乙腈)∶V(水)=3∶7為流動相,建立瞭兩種農藥的標準麯線,結果錶明在0.05~5μg· mL-1範圍內線性關繫均良好。進行樣品加標迴收實驗,用乙腈提取,C18固相萃取柱淨化,上述條件進行下分析,0.1,0.5,1.5 mg· kg-1三箇加標濃度迴收率均在75%~110%,變異繫數<5%,準確性和穩定性都較好,方法最低定量限0.01μg· g-1,完全可以用于實際樣品的檢測。
경과자외소묘학정필충람화정충미적최대자외흡수파장분별위270화246 nm,통과개변기비례우화출봉시간화분리도,학정V(을정)∶V(수)=3∶7위류동상,건립료량충농약적표준곡선,결과표명재0.05~5μg· mL-1범위내선성관계균량호。진행양품가표회수실험,용을정제취,C18고상췌취주정화,상술조건진행하분석,0.1,0.5,1.5 mg· kg-1삼개가표농도회수솔균재75%~110%,변이계수<5%,준학성화은정성도교호,방법최저정량한0.01μg· g-1,완전가이용우실제양품적검측。
The maximum absorption wavelength of imidacloprid and nitenpyram detected by UV spectrophotometer were 270 nm and 246 nm.To get optimum retention time and separation , the mobile phase should be acetonitrile and water ( V/V, 3∶7 ) .Standard curves of two pesticides were developed , which fit a linear regression ranging from 0.05 to 5 μg· mL-1 .After extracted by homogenate with acetonitrile and purified by C 18 SPE column, the recovery rates of the two pesticides were 75%~110% at the levels of 0.1mg· kg -1 , 0.5mg· kg-1 and 1.5mg· kg -1 with a RSD less than 5%, which showed a good accuracy and stability .This method with a limit of quantification ( LOQ) of 0.01μg· g-1 could be used in the practical detections .