Xu X, Stewart J T
Department of Pharmaceutical and Biomedical Sciences, College of Pharmacy, The University of Georgia, Athens 30602-2352, USA.
J Pharm Biomed Anal. 2000 Sep;23(4):735-43. doi: 10.1016/s0731-7085(00)00356-3.
Dopamine D-2 receptor antagonists' eticlopride and sulpiride were determined in serum using capillary electrophoresis with cyclodextrin additives. Chiral resolution of S(-) and R(+) sulpiride and eticlopride were achieved using 2% sulfated-beta-cyclodextrin (S-beta-CD) in 20 mM citrate run buffer (pH 2.90). A 72-cm fused silica capillary operated in the reversed polarity mode voltage of 20 kV was used for the analysis. The analytes of interest were isolated from serum using a solid phase extraction procedure with recoveries in excess of 85% for all four enantiomers. The D-2 receptor antagonist (-) butaclamol was used as internal standard. The limits of detection were 0.3 and 0.1 microg/ml for S(-) and R(+) eticlopride and for S(-) and R(+) sulpiride, respectively, in 1 ml of serum. The limits of quantitation were 2 and 1 microg/ml for S(-) and R(+) eticlopride, and for S(-) and R(+) sulpiride, respectively. Calibration curves were linear over the 2-20 micro/ml range for eticlopride and 1-20 microg/ml range for sulpiride. The coefficients of determination were greater than 0.99 (n = 12 for eticlopride and n = 15 for sulpiride). Precision and accuracy of the method were 0.27-6.38 and 0.20-3.60% for S(-) eticlopride, 2.33-4.28 and 0.80-5.73%, for R(+) eticlopride, 3.46-6.84 and 0.80-4.26%, for S(-) sulpiride; and 4.71 -6.47 and 2.00-6.67%, for R(+)-sulpiride, respectively.
采用含环糊精添加剂的毛细管电泳法测定血清中的多巴胺D - 2受体拮抗剂依托必利和舒必利。在pH 2.90的20 mM柠檬酸盐运行缓冲液中使用2%硫酸化β - 环糊精（S - β - CD）实现了S(-)和R(+)舒必利及依托必利的手性拆分。分析采用一根72 cm的熔融石英毛细管，在20 kV的反相模式电压下运行。使用固相萃取程序从血清中分离出目标分析物，所有四种对映体的回收率均超过85%。D - 2受体拮抗剂(-)布他拉莫用作内标。在1 ml血清中，S(-)和R(+)依托必利以及S(-)和R(+)舒必利的检测限分别为0.3和0.1 μg/ml。S(-)和R(+)依托必利以及S(-)和R(+)舒必利的定量限分别为2和1 μg/ml。依托必利在2 - 20 μg/ml范围内校准曲线呈线性，舒必利在1 - 20 μg/ml范围内校准曲线呈线性。测定系数大于0.99（依托必利n = 12，舒必利n = 15）。该方法对于S(-)依托必利的精密度和准确度分别为0.27 - 6.38%和0.20 - 3.60%，对于R(+)依托必利为2.33 - 4.28%和0.80 - 5.73%，对于S(-)舒必利为3.46 - 6.84%和0.80 - 4.26%，对于R(+)舒必利为4.71 - 6.47%和2.00 - 6.67%。
