农药学学报
農藥學學報
농약학학보
CHINESE JOURNAL OF PESTICIDE SCIENCE
2009年
4期
456-461
,共6页
王蒙岑%吴慧明%刘少颖%求银园%朱烨操%朱国念
王矇岑%吳慧明%劉少穎%求銀園%硃燁操%硃國唸
왕몽잠%오혜명%류소영%구은완%주엽조%주국념
乙螨唑%柑桔%土壤%残留%消解动态%超高效液相色谱-串联质谱
乙螨唑%柑桔%土壤%殘留%消解動態%超高效液相色譜-串聯質譜
을만서%감길%토양%잔류%소해동태%초고효액상색보-천련질보
etoxazole%orange%soil%residues%decline dynamics%UPLC-MS/MS
应用超高效液相色谱-串联质谱(UPLC-MS/MS)建立了乙螨唑在柑桔和土壤中残留的分析方法,并研究了田间试验条件下乙螨唑在柑桔和土壤中的消解动态.样品采用乙腈提取,硅胶柱净化,UPLC-MS/MS检测,外标法(ESTD)定量.在0.002 ~1 mg/L质量浓度范围内,乙螨唑的仪器响应值与质量浓度呈良好线性关系,相关系数为0.998 9.该方法的最小检出量为6.0×10~(-6) μg,乙螨唑在柑桔和土壤中的最低检测浓度均为0.002 mg/kg.当乙螨唑在柑桔和土壤中的添加水平为0.002 ~1 mg/kg时,平均回收率为87.3% ~98.4%,相对标准偏差在5.5% ~8.6%之间.消解动态试验表明,乙螨唑的消解动态曲线符合一级动力学方程,在柑桔和土壤中的半衰期分别为5.6 ~7.6 d 和 5.3 ~8.6 d.
應用超高效液相色譜-串聯質譜(UPLC-MS/MS)建立瞭乙螨唑在柑桔和土壤中殘留的分析方法,併研究瞭田間試驗條件下乙螨唑在柑桔和土壤中的消解動態.樣品採用乙腈提取,硅膠柱淨化,UPLC-MS/MS檢測,外標法(ESTD)定量.在0.002 ~1 mg/L質量濃度範圍內,乙螨唑的儀器響應值與質量濃度呈良好線性關繫,相關繫數為0.998 9.該方法的最小檢齣量為6.0×10~(-6) μg,乙螨唑在柑桔和土壤中的最低檢測濃度均為0.002 mg/kg.噹乙螨唑在柑桔和土壤中的添加水平為0.002 ~1 mg/kg時,平均迴收率為87.3% ~98.4%,相對標準偏差在5.5% ~8.6%之間.消解動態試驗錶明,乙螨唑的消解動態麯線符閤一級動力學方程,在柑桔和土壤中的半衰期分彆為5.6 ~7.6 d 和 5.3 ~8.6 d.
응용초고효액상색보-천련질보(UPLC-MS/MS)건립료을만서재감길화토양중잔류적분석방법,병연구료전간시험조건하을만서재감길화토양중적소해동태.양품채용을정제취,규효주정화,UPLC-MS/MS검측,외표법(ESTD)정량.재0.002 ~1 mg/L질량농도범위내,을만서적의기향응치여질량농도정량호선성관계,상관계수위0.998 9.해방법적최소검출량위6.0×10~(-6) μg,을만서재감길화토양중적최저검측농도균위0.002 mg/kg.당을만서재감길화토양중적첨가수평위0.002 ~1 mg/kg시,평균회수솔위87.3% ~98.4%,상대표준편차재5.5% ~8.6%지간.소해동태시험표명,을만서적소해동태곡선부합일급동역학방정,재감길화토양중적반쇠기분별위5.6 ~7.6 d 화 5.3 ~8.6 d.
A rapid,accurate and sensitive method has been developed to determine etoxazole residues in orange and soil by UPLC-MS/MS.The decline dynamics of etoxazole residues in orange and soil were studied under the conditon of field experiment.The samples were extracted by acetonitrile,followed by clean-up on silica gel cartridge and analyzed by UPLC-MS/MS.External reference method was used for quantitative determination.The linearity was satisfied (r=0.998 9) in the concentration range of 0.002-1 mg/L.The limit of detection was 6.0×10~(-6) μg,and the limit of quantification in orange and soil was 0.002 mg /kg.The average fortified recoveries varied from 87.3% to 98.4% with the coefficient of variation of 5.5%- 8.6%.The study of residue dynamics indicated that the curve of decline accorded with the first-order kinetics equation,and the half-life of etoxazole in orange and soil were 5.6- 7.6 d and 5.3- 8.6 d,respectively.