CAJ | 학술논문

研究和建立了氟啶虫胺腈在土壤、棉籽和棉叶中的高效液相色谱检测方法，并在天津和杭州两地开展了氟啶虫胺腈在棉花中的田间残留试验研究。样品采用乙腈提取，正己烷萃取，氟罗里硅土柱层析净化，正己烷/丙酮（体积比6：4）混合液洗脱，减压浓缩至干，甲醇定容，高效液相色谱配可变波长紫外检测器进行检测。当分别在空白土壤、棉籽和棉叶样品中添加浓度为0.05~2.5 mg·kg-1的氟啶虫胺腈标准品时，其平均添加回收率在76.81%~94.43%之间，相对标准偏差（R SD）在0.54%~7.20%之间；氟啶虫胺腈的最小检出量为1 ng，在所有样品中的最低检出浓度均为0.05 mg·kg-1。田间残留试验结果表明，氟啶虫胺腈在土壤和棉叶中的消解规律符合一级动力学模型Ct=C0e-kt，消解半衰期分别为1.36~5.10 d和6.13~9.37 d。最终残留试验结果表明，在棉花田手动喷雾施用50%氟啶虫胺腈水分散粒剂，按推荐剂量和1.5倍推荐剂量施药，兑水喷雾处理2~3次，每次施药间隔7 d，在距最后1次施药7、14 d和21 d时，氟啶虫胺腈在棉籽和土壤中的残留量均小于方法最低检出浓度0.05 mg·kg-1。
연구화건립료불정충알정재토양、면자화면협중적고효액상색보검측방법，병재천진화항주량지개전료불정충알정재면화중적전간잔류시험연구。양품채용을정제취，정기완췌취，불라리규토주층석정화，정기완/병동（체적비6：4）혼합액세탈，감압농축지간，갑순정용，고효액상색보배가변파장자외검측기진행검측。당분별재공백토양、면자화면협양품중첨가농도위0.05~2.5 mg·kg-1적불정충알정표준품시，기평균첨가회수솔재76.81%~94.43%지간，상대표준편차（R SD）재0.54%~7.20%지간；불정충알정적최소검출량위1 ng，재소유양품중적최저검출농도균위0.05 mg·kg-1。전간잔류시험결과표명，불정충알정재토양화면협중적소해규률부합일급동역학모형Ct=C0e-kt，소해반쇠기분별위1.36~5.10 d화6.13~9.37 d。최종잔류시험결과표명，재면화전수동분무시용50%불정충알정수분산립제，안추천제량화1.5배추천제량시약，태수분무처리2~3차，매차시약간격7 d，재거최후1차시약7、14 d화21 d시，불정충알정재면자화토양중적잔류량균소우방법최저검출농도0.05 mg·kg-1。
An analytical method with high performance liquid chromatography(HPLC)was established for determining sulfoxaflor residue in soil, cotton seeds and cotton leaves. The field residue decline study and final residue trials of sulfoxaflor in cotton in Tianjin City and Hangzhou City, were designed. The samples were extracted with acetonitrile, partitioned by n-hexane, purified using Florisil column, and de-termined by HPLC equipped with a variable wavelength detector(VWD). The results showed that when the spiked levels were 0.05 mg·kg-1 to 2.5 mg·kg-1, the average recovery of sulfoxaflor ranged from 76.81%to 94.43%with relative standard deviation (RSD)of 0.54%to 7.20%;the limit of detection(LOD)of sulfoxaflor was 1 ng, and the limit of quantification(LOQ)was 0.05 mg·kg-1 in soil, cotton seeds and cotton leaves. The degradation of sulfoxaflor in soil and cotton leaves could be described with an equation:Ct=C0e-kt. The half-life of sulfoxaflor were 1.36~5.10 d and 6.13~9.37 d in soil and cotton leaves, respectively. The wheat was sprayed with 50%water dispersible granule(WDG)at dosage 0.6~0.9 g·30 m-2(2~3 times)at full-bloom stage, the interval period was 7 d, the final residues of sulfoxaflor were lower than LOQ in soil and cotton seeds.