CAJ | 학술논문

建立了一种同步分析水稻和土壤中福美双和甲霜灵残留的分散固相萃取-高效液相色谱-串联质谱（ HPLC-MS／MS ）检测方法。样品经乙腈提取，PSA、C18吸附剂净化，C18色谱柱分离，0.2％甲酸水-乙腈等度洗脱，质谱采用电喷雾正离子（ ESI+）模式电离，多反应离子监测模式定性分析，基质匹配标准曲线外标法定量。结果表明：在1～500μg／L浓度范围内，不同基质中的福美双和甲霜灵的线性相关系数均大于0.991。在0.01～1.5 mg／kg添加水平范围内，土壤、水稻植株、稻壳和糙米样品中福美双和甲霜灵的日内平均回收率为76％～104％，日内相对标准偏差（ RSD）为1.2％～13.2％（ n＝5）；日间平均回收率为74％～102％，日间RSD为2.8％～10.4％（n＝5）。该方法简单、快速、灵敏度及准确度高，能够满足水稻及土壤中福美双和甲霜灵残留量的检测要求。
건립료일충동보분석수도화토양중복미쌍화갑상령잔류적분산고상췌취-고효액상색보-천련질보（ HPLC-MS／MS ）검측방법。양품경을정제취，PSA、C18흡부제정화，C18색보주분리，0.2％갑산수-을정등도세탈，질보채용전분무정리자（ ESI+）모식전리，다반응리자감측모식정성분석，기질필배표준곡선외표법정량。결과표명：재1～500μg／L농도범위내，불동기질중적복미쌍화갑상령적선성상관계수균대우0.991。재0.01～1.5 mg／kg첨가수평범위내，토양、수도식주、도각화조미양품중복미쌍화갑상령적일내평균회수솔위76％～104％，일내상대표준편차（ RSD）위1.2％～13.2％（ n＝5）；일간평균회수솔위74％～102％，일간RSD위2.8％～10.4％（n＝5）。해방법간단、쾌속、령민도급준학도고，능구만족수도급토양중복미쌍화갑상령잔류량적검측요구。
A rapid analytical method for the simultaneous determination of thiram and metalaxyl in paddy soil,rice plant,rice husk and brown rice was developed using dispersive solid phase extraction and high performance liquid chromatography-tandem mass spectrometry( HPLC-MS/MS ). The analytes was extracted by acetonitrile and cleaned up by PSA and C18 ,and then separated on a reversed phase C18 column using an isocratic elution program of 0. 2% aqueous formic acid and acetonitrile. Qualitative analysis was performed with electrospray ionization in positive mode( ESI+)under multiple reaction monitoring( MRM)mode. Matrix-matched calibrations were respectively used to quantify the residue concentrations. In the concentration range of 1 -500 μg/L,the matrix-matched calibration curves showed good linearity with correlation coefficients ﹥0. 991 . Intra-day mean recoveries of thiram and metalaxyl in different matrices were found between 76% and 104% at 0. 01 -1. 5 mg/kg,with relative standard deviations(RSD)of 1. 2% -13. 2%(n=5). Inter-day mean recoveries of thiram and metalaxyl were found between 74% and 102% with RSD of 2. 8% -10. 4% at 0. 01-1. 5 mg/kg( n=5 ). The method is simple,rapid,sensitive and accurate,which can meet the detection requirements of thiram and metalaxyl residues in rice samples and soil.