江西农业大学学报
江西農業大學學報
강서농업대학학보
ACTA AGRICULTURAE UNIVERSITATIS JIANGXIENSIS
2014年
2期
326-331
,共6页
汤凯洁%周志娥%余瑞龙%陈尚卫
湯凱潔%週誌娥%餘瑞龍%陳尚衛
탕개길%주지아%여서룡%진상위
磺酰脲除草剂%吡嘧磺隆%固相萃取%梯度洗脱%土壤
磺酰脲除草劑%吡嘧磺隆%固相萃取%梯度洗脫%土壤
광선뇨제초제%필밀광륭%고상췌취%제도세탈%토양
sulfonylurea herbicides%pyrazosulfuron-ethyl%solid-phase extraction%gradient elution%soil
研究了高效液相色谱法同时分离测定烟嘧磺隆、甲磺隆、苯磺隆、苄嘧磺隆和吡嘧磺隆等5种不同磺酰脲类除草剂的色谱条件。流动相A为V(乙腈)∶V(水)=20∶80,流动相B为V(乙腈)∶V(水)=80∶20,以0.01%磷酸调pH,比较了3种不同的梯度洗脱条件的分离效果。结果表明:梯度3分离效果最佳,流速为0.8 mL/min,检测波长λ=241 nm,柱温为30℃,5种磺酰脲在18 min达到了基线分离。浓度与峰面积呈良好的线性关系( R2=0.9982~0.9998),对标样的检测限在0.02~0.09μg/mL。应用此方法测定加标土壤样品中5种磺酰脲类除草剂的残留量,添加量在3.5 mg/kg时的回收率在89.1%~98.6%。
研究瞭高效液相色譜法同時分離測定煙嘧磺隆、甲磺隆、苯磺隆、芐嘧磺隆和吡嘧磺隆等5種不同磺酰脲類除草劑的色譜條件。流動相A為V(乙腈)∶V(水)=20∶80,流動相B為V(乙腈)∶V(水)=80∶20,以0.01%燐痠調pH,比較瞭3種不同的梯度洗脫條件的分離效果。結果錶明:梯度3分離效果最佳,流速為0.8 mL/min,檢測波長λ=241 nm,柱溫為30℃,5種磺酰脲在18 min達到瞭基線分離。濃度與峰麵積呈良好的線性關繫( R2=0.9982~0.9998),對標樣的檢測限在0.02~0.09μg/mL。應用此方法測定加標土壤樣品中5種磺酰脲類除草劑的殘留量,添加量在3.5 mg/kg時的迴收率在89.1%~98.6%。
연구료고효액상색보법동시분리측정연밀광륭、갑광륭、분광륭、변밀광륭화필밀광륭등5충불동광선뇨류제초제적색보조건。류동상A위V(을정)∶V(수)=20∶80,류동상B위V(을정)∶V(수)=80∶20,이0.01%린산조pH,비교료3충불동적제도세탈조건적분리효과。결과표명:제도3분리효과최가,류속위0.8 mL/min,검측파장λ=241 nm,주온위30℃,5충광선뇨재18 min체도료기선분리。농도여봉면적정량호적선성관계( R2=0.9982~0.9998),대표양적검측한재0.02~0.09μg/mL。응용차방법측정가표토양양품중5충광선뇨류제초제적잔류량,첨가량재3.5 mg/kg시적회수솔재89.1%~98.6%。
A high-performance liquid chromatography ( HPLC) method for separation and determination of nicosulfuron,metsulfuron-methyl,tribenuron-methyl,bensulfuron-methyl and pyrazosulfuron-ethyl was studied.The mixture of (A) acetonitrile-water containing 0.01%phosphoric acid (20 ∶80,V/V) and (B) acetonitrile-water (80∶20,V/V) were used as the mobile phase;the effects of three gradient elution proce-dures were compared .The results showed that gradient 3 had the best separation effect .The flow rate was 0.8 mL/min,the detection wavelength was 241 nm,the column temperature was 30 ℃,the baseline sparation was obtained for the five different sulfonylurea herbicides at 18 min.The concentration and peak area showed a good linear relationship ( R2=0.998 2-0.999 8) ,the limits of detection ranged from 0.02-0.07 μg/mL.When this method was used to determine the residues of the five sulfonylurea herbicides in the soil sample ,the recoveries ranged from 89.09%to 98.62 %when 3.5μg/mL standard solution was spiked .