Kline W F, Matuszewski B K, Bayne W F
Merck Sharp & Dohme Research Laboratories, West Point, PA 19486.
J Chromatogr. 1990 Dec 14;534:139-49. doi: 10.1016/s0378-4347(00)82156-8.
A sensitive (5 ng/ml) method for the determination of 4-amino-1-hydroxybutane-1,1-bisphosphonic acid in human urine is described. The procedure includes (1) the isolation of the drug from urine by co-precipitation of its calcium salt with endogenous phosphates in the presence of base, (2) a solid-phase anion-exchange sample clean-up and (3) automated pre-column derivatization of the primary amino group with 2,3-naphthalene dicarboxyaldehyde-cyanide reagent followed by fluorescence detection of the N-substituted cyanobenz[f]isoindole derivative. The derivative of the drug was synthesized and its spectral and fluorescence properties were evaluated. The fluorescence quantum efficiency was determined to be 0.82 in the mobile phase used for the assay. The derivative is also capable of accepting energy in an oxalate ester-hydrogen peroxide chemiluminescence system.
描述了一种灵敏的（5纳克/毫升）测定人尿中4-氨基-1-羟基丁烷-1,1-二膦酸的方法。该程序包括：（1）在碱存在下，通过其钙盐与内源性磷酸盐共沉淀从尿中分离药物；（2）固相阴离子交换样品净化；（3）用2,3-萘二甲醛-氰化物试剂对伯氨基进行自动柱前衍生，随后对N-取代的氰基苯并[f]异吲哚衍生物进行荧光检测。合成了该药物的衍生物并评估了其光谱和荧光性质。在用于测定的流动相中，荧光量子效率测定为0.82。该衍生物在草酸酯-过氧化氢化学发光系统中也能够接受能量。
