Hariharan M, VanNoord T, Kindt E K, Tandon R
Department of Psychiatry, University of Michigan Medical School, Ann Arbor 48109-0656.
Ther Drug Monit. 1991 Jan;13(1):79-85. doi: 10.1097/00007691-199101000-00012.
A novel, simple, and very sensitive liquid-chromatographic assay with a coulometric detector has been developed for quantitating cis-thiothixene (CTX) in human plasma. A reverse phase, 5-microns cyano column (25 x 0.46 cm), a mobile phase of phosphate buffer (pH 2.5) and acetonitrile (40/60 by vol), and a coulometric detector are used for the separation of CTX, and the internal standard, trifluoperazine. CTX and trifluoperazine are extracted from alkalinized plasma into n-pentane-isopropanol (95/5 by vol) and purified by back extraction into perchloric acid. The optimum oxidation potential for the analytes is +0.8 V versus an Ag/AgCl electrode. The detection limit for CTX is 200 pg using 1 mL of plasma and CTX concentrations are linear from 0 to 40 micrograms/L. The average interassay CV is 9%, and the mean recovery is 99% relative to the internal standard. Possible interferences from various psychiatric and common drugs in the assay have been studied. The assay method was validated by determining the concentration of CTX in the plasma of 100 schizophrenic patients.
已开发出一种新颖、简单且灵敏度极高的液相色谱法，采用库仑检测器来定量测定人血浆中的顺式硫代噻吨（CTX）。使用反相5微米氰基柱（25×0.46厘米）、磷酸盐缓冲液（pH 2.5）与乙腈（体积比40/60）的流动相以及库仑检测器来分离CTX和内标物三氟拉嗪。CTX和三氟拉嗪从碱化血浆中萃取到正戊烷 - 异丙醇（体积比95/5）中，并通过反萃取到高氯酸中进行纯化。相对于银/氯化银电极，分析物的最佳氧化电位为+0.8伏。使用1毫升血浆时，CTX的检测限为200皮克，CTX浓度在0至40微克/升范围内呈线性。平均批间变异系数为9%，相对于内标物的平均回收率为99%。已研究了该测定法中各种精神科药物和常用药物可能产生的干扰。通过测定100例精神分裂症患者血浆中CTX的浓度对该测定方法进行了验证。
