Xu X, Pang K S
Faculty of Pharmacy, University of Toronto, Ontario, Canada.
J Chromatogr. 1987 Sep 25;420(2):313-27. doi: 10.1016/0378-4347(87)80187-1.
A high-performance liquid chromatographic (HPLC) assay is described for the determination of salicylamide (SAM) and its metabolites in biological fluids obtained from an in situ rat liver preparation and rat in vivo. SAM and its six metabolites, salicylamide sulphate, salicylamide glucuronide, gentisamide (GAM), gentisamide 2-sulphate, gentisamide 5-sulphate and gentisamide 5-glucuronide, were separated on a mu Bondapak C18 column with 0.085 M potassium dihydrogenphosphate pH 3.35, as mobile phase and by using a flow gradient. Enriched recovery of SAM and GAM from blood was achieved by extraction followed by a second HPLC procedure with a mobile phase consisting of acetic acid and methanol. Furthermore, the reproducibility and the stability of the samples under assay conditions were investigated.
本文描述了一种高效液相色谱（HPLC）分析方法，用于测定从原位大鼠肝脏制剂和大鼠体内获得的生物流体中的水杨酰胺（SAM）及其代谢物。SAM及其六种代谢物，即硫酸水杨酰胺、水杨酰胺葡萄糖醛酸苷、龙胆酰胺（GAM）、龙胆酰胺2-硫酸盐、龙胆酰胺5-硫酸盐和龙胆酰胺5-葡萄糖醛酸苷，在μ Bondapak C18柱上分离，以0.085 M磷酸二氢钾pH 3.35作为流动相，并采用流动梯度。通过萃取，然后用由乙酸和甲醇组成的流动相进行第二次HPLC程序，实现了从血液中富集回收SAM和GAM。此外，还研究了样品在分析条件下的重现性和稳定性。
