Siluveru M, Stewart J T
Department of Medicinal Chemistry, College of Pharmacy, University of Georgia, Athens 30602-2352, USA.
J Pharm Biomed Anal. 1996 Dec;15(3):389-92. doi: 10.1016/s0731-7085(96)01872-9.
A chiral HPLC method was developed for the quantitation of R(-)- and S(+)-prilocaine in human serum. The method involves sensitive and selective detection of R(-)- and S(+)-prilocaine using normal-phase chiral HPLC on a pirkle-type naphthyl ethylamine stationary phase (Sumichiral OA-4700, 250 mm x 4 mm i.d.) at ambient temperature with a flow rate of 0.8 ml min-1. A sample clean-up procedure was used for isolation of the analytes of interest from human serum using Bond-Elut C18 columns with high recovery and selectivity. The detection limits were 4 ng ml-1 for R-prilocaine and 5 ng ml-1 for S-prilocaine. The limits of quantitation were 10 ng ml-1 for both enantiomers. Linear calibration curves in the 10-1000 ng ml-1 range showed good coefficients of determination > 0.999 (n = 3). Precision and accuracy of the method were within 4-5.8% and 1.5-4.8% respectively for R(-)-prilocaine, and 2.8-5.7% and 3.2-5.2% respectively for S(+)-prilocaine.
建立了一种手性高效液相色谱法用于定量测定人血清中R(-)-和S(+)-丙胺卡因。该方法包括在室温下，使用Pirkle型萘基乙胺固定相（Sumichiral OA-4700，250 mm×4 mm内径），以0.8 ml min-1的流速通过正相手性高效液相色谱法灵敏且选择性地检测R(-)-和S(+)-丙胺卡因。采用样品净化程序，使用Bond-Elut C18柱从人血清中分离出目标分析物，回收率高且选择性好。R-丙胺卡因的检测限为4 ng ml-1，S-丙胺卡因的检测限为5 ng ml-1。两种对映体的定量限均为10 ng ml-1。在10-1000 ng ml-1范围内的线性校准曲线显示，测定系数良好，R(-)-丙胺卡因的测定系数>0.999（n = 3），S(+)-丙胺卡因的测定系数分别在4-5.8%和1.5-4.8%之间，以及2.8-5.7%和3.2-5.2%之间。
