Krause R T
J Assoc Off Anal Chem. 1985 Jul-Aug;68(4):726-33.
A liquid chromatographic (LC) multiresidue method for determining residues of N-methylcarbamate insecticides in crops was collaboratively studied in 6 laboratories. Methanol and a mechanical ultrasonic homogenizer are used to extract the carbamates. Water-soluble plant coextractives and nonpolar plant lipid materials are removed from the carbamate residues by liquid-liquid partitioning. Additional crop coextractives (e.g., carotenes, chlorophylls) are removed with a Nuchar SN-silanized Celite column. The carbamate residues are then separated on a reverse phase LC column, using an acetonitrile-water gradient mobile phase. Eluted residues are detected by an in-line post-column fluorometric detection technique. Seven carbamates and 2 carbamate metabolites were included in the collaborative study. Each collaborator determined all the carbamates at 2 levels (approximately 0.05 ppm and United States tolerance) in blind duplicate samples of grapes and potatoes. Fortified and control samples were analyzed. Repeatability coefficients of variation for all the carbamates on the 2 crops averaged 4.7% and ranged from 2.4 to 7.1%. Reproducibility coefficients of variation for all the carbamates on the 2 crops averaged 8.7% and ranged from 5.3 to 12.4%. Accuracy, measured by comparison with fortification values, averaged 95% and ranged from 79 to 103%. The estimated limit of quantitation is 0.01 ppm. The method has been adopted official first action.
一个用于测定农作物中氨基甲酸酯类杀虫剂残留量的液相色谱（LC）多残留方法在6个实验室进行了协同研究。使用甲醇和机械超声均质器提取氨基甲酸酯类。通过液-液分配从氨基甲酸酯类残留中去除水溶性植物共提取物和非极性植物脂质材料。用Nuchar SN硅烷化硅藻土柱去除其他农作物共提取物（如胡萝卜素、叶绿素）。然后使用乙腈-水梯度流动相在反相LC柱上分离氨基甲酸酯类残留。通过在线柱后荧光检测技术检测洗脱的残留。协同研究中包括7种氨基甲酸酯类和2种氨基甲酸酯类代谢物。每位协作人员在葡萄和土豆的盲法双份样品中，以2个水平（约0.05 ppm和美国容许量）测定所有氨基甲酸酯类。对加标样品和对照样品进行了分析。2种作物上所有氨基甲酸酯类的重复性变异系数平均为4.7%，范围为2.4%至7.1%。2种作物上所有氨基甲酸酯类的再现性变异系数平均为8.7%，范围为5.3%至12.4%。与加标值比较测得的准确度平均为95%，范围为79%至103%。估计定量限为0.01 ppm。该方法已被采用为官方首次行动方法。
