Szulc M E, Krull I S
Barnett Institute, Northeastern University, Boston, Massachusetts 02115.
Biomed Chromatogr. 1992 Nov-Dec;6(6):269-77. doi: 10.1002/bmc.1130060605.
Several polymer-bound o-nitrobenzophenone reagents containing different detector-sensitive tags have been combined in the same reactor for the on-line derivatization of amine samples. The formation of multiple derivatives allows numerous opportunities for quantitation from the same injection, and also allows improved identification from the retention times of the multiple derivatives. Changing the reaction conditions changes the ratio of the products formed, so that changes in the ratio of peak heights and areas can also be used for analyte identification. In this work, propylamine was derivatized in acetonitrile on-line, precolumn. Changing the reaction conditions, of reaction time, temperature, solvent, presence of catalyst and the components of the reactor, changed the ratio of the derivatives formed. These changes in product formation with changing reaction conditions were applied to the identification and quantitation of amphetamine and methamphetamine in urine. The drugs were identified by the retention times of their derivatives, the ratio of the peak areas of the derivatives and the change in the ratios after changing reaction conditions. Each derivative was also used for quantitation of levels of spiked concentrations of amphetamine and methamphetamine, with relative errors less than 8%.
几种含有不同检测器敏感标签的聚合物结合邻硝基二苯甲酮试剂已被组合在同一反应器中，用于胺类样品的在线衍生化。多种衍生物的形成使得在同一次进样中有大量定量机会，同时也能通过多种衍生物的保留时间进行更准确的鉴定。改变反应条件会改变所形成产物的比例，因此峰高和峰面积比例的变化也可用于分析物鉴定。在这项工作中，丙胺在乙腈中进行在线柱前衍生化。改变反应时间、温度、溶剂、催化剂的存在以及反应器的组成等反应条件，会改变所形成衍生物的比例。这些随着反应条件变化而产生的产物形成变化被应用于尿液中苯丙胺和甲基苯丙胺的鉴定和定量。通过衍生物的保留时间、衍生物峰面积的比例以及改变反应条件后比例的变化来鉴定药物。每种衍生物还用于定量苯丙胺和甲基苯丙胺加标浓度水平，相对误差小于8%。
