Wigfield Y Y, Gurprasad N P, Lanouette M, Ripley S
Agriculture Canada, Food Production and Inspection Branch, Ottawa, Ontario.
J Assoc Off Anal Chem. 1987 Sep-Oct;70(5):792-6.
A new method is described to determine trace quantities of N-nitrosodiethanolamine (NDElA) in aqueous diethanolamine (DElA) formulations and in oil solutions of dinoseb. A formate anion-exchange column is used in series with a cation-exchange column if there is DElA in the formulation. The eluate is then passed through a Clin Elut column. Depending on the concentration of NDElA in the sample, a packed silica-gel column is used to purify the extract further. This extract is analyzed on a liquid chromatograph coupled with a thermal energy analyzer (LC/TEA), using a mixture of methanol-hexane-methylene chloride containing 0.1% acetic acid (8 + 56 + 35) as the mobile phase. This solvent system gives good separation of NDElA from trace quantities of dinoseb remaining in the extract. The NDElA is also converted to the trimethylsilyl derivative and analyzed by gas chromatograph coupled with a mass spectrometer (GC/MS). Analyses of 11 commercial samples of dinoseb diethanolamine salt showed NDElA levels of 116-2409 ppm expressed relative to the weight of dinoseb. In contrast, analyses of 2 samples of organic solutions of technical dinoseb showed NDElA levels to be nondetectable and 0.3 ppm, respectively. Limit of detection by LC/TEA is 6.5 ng (0.5 ppm), and by GC/MS it is 0.02 ng (0.15 ppm). Recoveries from samples spiked at 0.514-1664 ppm range from 92.2 to 105.2%.
本文描述了一种测定二乙醇胺（DElA）水性制剂和地乐酚油溶液中痕量N-亚硝基二乙醇胺（NDElA）的新方法。如果制剂中存在DElA，则使用甲酸根阴离子交换柱与阳离子交换柱串联。然后将洗脱液通过Clin Elut柱。根据样品中NDElA的浓度，使用填充硅胶柱进一步纯化提取物。该提取物在与热能分析仪联用的液相色谱仪（LC/TEA）上进行分析，使用含有0.1%乙酸（8 + 56 + 35）的甲醇-己烷-二氯甲烷混合物作为流动相。该溶剂系统能将NDElA与提取物中残留的痕量地乐酚很好地分离。NDElA还被转化为三甲基硅烷基衍生物，并通过与质谱仪联用的气相色谱仪（GC/MS）进行分析。对11个地乐酚二乙醇胺盐商业样品的分析表明，相对于地乐酚的重量，NDElA含量为116 - 2409 ppm。相比之下，对2个工业用地乐酚有机溶液样品的分析表明，NDElA含量分别为未检出和0.3 ppm。LC/TEA的检测限为6.5 ng（0.5 ppm），GC/MS的检测限为0.02 ng（0.15 ppm）。在0.514 - 1664 ppm范围内加标样品的回收率为92.2%至105.2%。
