Aboul-Enein Hassan Y, Hefnawy Mohamed M
Pharmaceutical Analysis Laboratory, Biological and Medical Research Department (MBC-03), King Faisal Specialist Hospital and Research Centre, P.O. Box 3354, Riyadh 11211, Saudi Arabia.
Chirality. 2004 Mar;16(3):147-52. doi: 10.1002/chir.20001.
An enantioseparation of the antipsychotic drug butaclamol in human plasma by high-performance liquid chromatography (HPLC) with solid phase extraction is presented. The separation was achieved on the vancomycin macrocyclic antibiotic chiral stationary phase (CSP) Chirobiotic V with a polar ionic mobile phase (PIM) consisting of methanol : glacial acetic acid : triethylamine (100:0.2:0.05, v/v/v) at a flow rate of 0.5 ml/min. The detection wavelength was 262 nm. Bond Elut C18 solid phase extraction cartridges were used in the sample preparation of butaclamol samples from plasma. The method was validated over the range of 100-3,000 ng/ml for each enantiomer concentration (R(2) > 0.999). Recoveries for (+)- and (-)-butaclamol were in the range of 94-104% at the 300-2,500 ng/ml level. The method proved to be precise (within-run precision ranged from 1.1-2.6% and between-run precision ranged from 1.9-3.2%) and accurate (within-run accuracies ranged from 1.5-5.8% and between-run accuracies ranged from 2.7-7.7%). The limit of quantitation (LOQ) and limit of detection (LOD) for each enantiomer in human plasma were 100 ng/ml and 50 ng/ml, respectively.
本文介绍了一种采用高效液相色谱法（HPLC）结合固相萃取技术对人血浆中抗精神病药物布他拉莫进行对映体分离的方法。该分离在万古霉素大环抗生素手性固定相（CSP）Chirobiotic V上实现，流动相为极性离子流动相（PIM），由甲醇：冰醋酸：三乙胺（100:0.2:0.05，v/v/v）组成，流速为0.5 ml/min。检测波长为262 nm。在从血浆中制备布他拉莫样品时，使用了Bond Elut C18固相萃取柱。该方法在每种对映体浓度100 - 3000 ng/ml范围内进行了验证（R(2) > 0.999）。在300 - 2500 ng/ml水平下，(+)-和(-)-布他拉莫的回收率在94 - 104%范围内。该方法被证明具有精密度（批内精密度范围为1.1 - 2.6%，批间精密度范围为1.9 - 3.2%）和准确度（批内准确度范围为1.5 - 5.8%，批间准确度范围为2.7 - 7.7%）。人血浆中每种对映体的定量限（LOQ）和检测限（LOD）分别为100 ng/ml和50 ng/ml。
