Siluveru M, Stewart J T
Department of Medicinal Chemistry, College of Pharmacy, University of Georgia, Athens 30602-2352, USA.
J Chromatogr B Biomed Sci Appl. 1997 Mar 7;690(1-2):359-62. doi: 10.1016/s0378-4347(96)00347-7.
A stereoselective high-performance liquid chromatography assay method was developed for the quantitation of R-(+)- and S-(-)-mepivacaine in human serum. The assay uses a Pirkle brush-type (S)-tert.-leucine, (R)-1-(alpha-naphthyl)ethylamine stationary phase (Sumichiral OA-4700, 250 x 4 mm I.D.) at ambient temperature with a mobile phase of hexane-ethylenedichloride-absolute methanol (85:10:5, v/v) for the separation of R-(+)- and S-(-)-mepivacaine. The eluents were monitored using UV detection at 220 nm. Isolation of the analytes from serum was performed using a 1-ml C18 solid-phase extraction cartridge with high recovery and selectivity. The detection limits were 100 ng/ml for each enantiomer and the limits of quantitation were 150 ng/ml for both enantiomers. Linear calibration curves in the 150-2400 ng/ml range showed good correlation coefficients (r > 0.9994, n = 3). Precision and accuracy of the method were within 2.1-5.3 and 2.0-3.6%, respectively, for R-(+)-mepivacaine and 2.7-5.7% and 1.7-4.2%, respectively, for S-(-)-mepivacaine.
建立了一种立体选择性高效液相色谱法，用于定量测定人血清中R-(+)-和S-(-)-甲哌卡因。该方法在环境温度下使用Pirkle刷型(S)-叔亮氨酸、(R)-1-(α-萘基)乙胺固定相（Sumichiral OA-4700，内径250×4 mm），流动相为己烷-二氯乙烷-无水甲醇（85:10:5，v/v），用于分离R-(+)-和S-(-)-甲哌卡因。使用紫外检测器在220 nm处监测洗脱液。采用1 ml C18固相萃取柱从血清中分离分析物，回收率高且选择性好。对映体的检测限均为100 ng/ml，定量限均为150 ng/ml。在150 - 2400 ng/ml范围内的线性校准曲线显示出良好的相关系数（r > 0.9994，n = 3）。该方法对R-(+)-甲哌卡因的精密度和准确度分别在2.1 - 5.3%和2.0 - 3.6%以内，对S-(-)-甲哌卡因分别在2.7 - 5.7%和1.7 - 4.2%以内。
