Lindberg R L, Pihlajamäki K K
J Chromatogr. 1984 Aug 10;309(2):369-74. doi: 10.1016/0378-4347(84)80044-4.
A selective high-performance liquid chromatographic method for the determination of bupivacaine in human serum is described. The technique is based on a single extraction of the drug from alkalinized serum with a mixture of hexane-isopropanol-chloroform. Desmethyldoxepin is used as internal standard. The chromatographic system consists of a home-packed Nucleosil C8 (10 microns) column; the mobile phase is acetonitrile--0.05 M potassium phosphate buffer (pH 3.3) (28:72, v/v). The method can accurately measure serum bupivacaine concentrations down to 20 micrograms/l using 500 microliters of sample. The coefficient of variation for intra-assay variability of bupivacaine is 2.1% (n = 13) and for inter-assay variability of bupivacaine 5.7% (n = 11) at 1.00 mg/l. The calibration graph is linear over the range 0.02-5.00 mg/l and the extraction efficiency is 91.8 +/- 3.8% (+/- S.D., n = 7). The method is accurate and sensitive for both clinical and pharmacokinetic studies on bupivacaine in man. The method is applied to the analysis of serum samples obtained from orthopaedic patients during both spinal and epidural analgesia.
本文描述了一种测定人血清中布比卡因的选择性高效液相色谱法。该技术基于用己烷 - 异丙醇 - 氯仿混合物从碱化血清中单次提取药物。去甲多虑平用作内标。色谱系统由自制填充的Nucleosil C8(10微米)柱组成;流动相为乙腈 - 0.05M磷酸钾缓冲液(pH 3.3)(28:72,v/v)。该方法使用500微升样品可准确测量低至20微克/升的血清布比卡因浓度。在1.00毫克/升时,布比卡因的批内变异系数为2.1%(n = 13),批间变异系数为5.7%(n = 11)。校准曲线在0.02 - 5.00毫克/升范围内呈线性,提取效率为91.8 +/- 3.8%(+/-标准差,n = 7)。该方法对布比卡因在人体的临床和药代动力学研究既准确又灵敏。该方法应用于分析骨科患者在脊髓和硬膜外镇痛期间采集的血清样本。