Briggle T V, Allen L M, Duncan R C, Pfaffenberger C D
J Assoc Off Anal Chem. 1981 Sep;64(5):1222-6.
A reverse phase high performance liquid chromatographic (HPLC) assay for the quantitative determination of cyanuric acid (CA) in urine and water is described. For purification, samples are passed through a pre-activated reverse phase C18 column. The effluent is dried by lyophilization, and the residue is reconstituted in hexane-washed water and then passed through a prewashed Dowex-1 column. The effluent is again dried by lyophilization, and the dry residue is extracted with hot dioxane. The solution is cooled to ambient temperature and centrifuged. The supernatant liquid is removed, dried under a nitrogen steam, and dissolved in water for final extraction by reverse phase chromatography. This effluent is dried, dissolved in the sodium phosphate monohydrate in methanol (pH 7.0) mobile phase, and injected into a pre-equilibrated chromatographic system. An external standard is used for quantification by peak height comparison. A sample of HPLC column effluent is collected, dried, dissolved in methanol, and used for mass spectrometric confirmation by a solid probe insert procedure. Average combined recovery determined at 1.0, 5.0 and 10.0 micrograms CA/mL is 103 +/- 3% with an average coefficient of variation of 8.6%. Standard deviations for the 3 concentration levels are 0.04, 0.58, and 0.76, respectively, with average precisions of 4.28, 10.92, and 7.61%. The limits of detection are approximately 0.05 micrograms/mL for urine and 0.1 micrograms/mL for swimming pool water. Recorder response to CA is linear over the concentration range 1-10 microgram/mL.
本文描述了一种用于定量测定尿液和水中氰尿酸（CA）的反相高效液相色谱（HPLC）分析方法。为进行纯化，样品通过预先活化的反相C18柱。流出物经冻干干燥，残留物用己烷洗涤水复溶，然后通过预先洗涤的Dowex - 1柱。流出物再次经冻干干燥，干燥的残留物用热二氧六环萃取。溶液冷却至室温并离心。去除上清液，在氮气流下干燥，并溶解于水中用于反相色谱的最终萃取。该流出物干燥后，溶解于甲醇中的磷酸二氢钠（pH 7.0）流动相中，并注入预先平衡的色谱系统。通过峰高比较使用外标进行定量。收集HPLC柱流出物的样品，干燥，溶解于甲醇中，并通过固体探针插入程序用于质谱确认。在1.0、5.0和10.0微克CA/mL下测定的平均合并回收率为103±3%，平均变异系数为8.6%。3个浓度水平的标准偏差分别为0.04、0.58和0.76，平均精密度分别为4.28%、10.92%和7.61%。尿液的检测限约为0.05微克/mL，游泳池水的检测限为0.1微克/mL。记录仪对CA的响应在1 - 10微克/mL的浓度范围内呈线性。
