CAJ | 학술논문

建立了用凝胶渗透色谱净化-高效液相色谱-串联质谱分析贝类等复杂样品中扑草净残留的方法。样品用乙腈超声提取，凝胶净化系统净化，收集10 min~18 min的流出液并进行在线浓缩，通过液相色谱柱（ZORBAX SB-C18柱）分离后进行质谱检测。扑草净标准溶液在0.5μg/L~20.0μg/L浓度范围内，药物峰面积与浓度呈良好的线性关系，其相关系数的平方（R2）为0.9998。在添加量为0.5μg/kg~10.0μg/kg时，平均回收率范围为70.83%~83.98%，相对标准偏差范围为3.05%~6.75%。该方法的检出限为0.07μg/kg，方法的灵敏度、准确度和精密度均符合农药残留检测的技术要求，适用贝类及其产品中农药残留的检测。
건립료용응효삼투색보정화-고효액상색보-천련질보분석패류등복잡양품중복초정잔류적방법。양품용을정초성제취，응효정화계통정화，수집10 min~18 min적류출액병진행재선농축，통과액상색보주（ZORBAX SB-C18주）분리후진행질보검측。복초정표준용액재0.5μg/L~20.0μg/L농도범위내，약물봉면적여농도정량호적선성관계，기상관계수적평방（R2）위0.9998。재첨가량위0.5μg/kg~10.0μg/kg시，평균회수솔범위위70.83%~83.98%，상대표준편차범위위3.05%~6.75%。해방법적검출한위0.07μg/kg，방법적령민도、준학도화정밀도균부합농약잔류검측적기술요구，괄용패류급기산품중농약잔류적검측。
A gel permeation chromatographic method was developed for the extraction of prometryn residues in shellfish and other complex samples of shellfish to liquid chromatography-tandem mass spectrometry. Samples were extracted by ultrasonic extraction with acetonitrile , purified by GPC , collecting the effluent for 10 min-18 min, then dried by a rotavapor. Chromatographic column of ZORBAX SB-C18 was applied, after the separation by liquid chromatography mass spectrometry. Good linearity (R2=0.999 8) was abserved between 0.5μg/L and 20.0μg/L for all the analytes. The recoveries and relative standard deviations (RSDs) were checked by spiking samples at the levels from 0.5μg/kg to 10.0μg/kg. The average recoveries were from 70.83%to 83.98%. The precision values expressed as RSD ranged from 3.05%to 6.75%. The detection limit of the prometryn detection of residues in complex samples was 0.07μg/kg. The sensitivity and accuracy of the method met the requirements of the multiple pesticide residues. This method was applicable to determine prometryn in shellfishes.