高效液相色谱-电化学检测法测定脑组织中鬼臼甲叉甙

报道了用甲醇－水－乙酸（５６４１３，体积比）为流动相，在ＨｙｐｅｒｓｉｌＯＤＳ柱上以愈创木酚甘油醚为内标，采用电化学检测器（ＥＣＤ）测定人体脑组织中鬼臼甲叉甙含量。回收率９２．８７％，最低检测浓度为０．１ｍｇ／Ｌ，鬼臼甲叉甙在０．１～１０．０ｍｇ／Ｌ范围内呈线性，工作电压０．７０Ｖ。同时还对脑瘤患者脑组织中正常部位和肿瘤部分中鬼臼甲叉甙含量进行了测定。

A High Performance Liquid Chromatographic Method for the Determination of Teniposide in Brain Tissue Using Electro Chemical Detection

A reversed-phase HPLC method for the determination of teniposide in brain tissue is described. Teniposide can be separated on a Hypersil ODS column with a mobile phase of methyl alcohol-water-acetic acid (56:41:3, V/V) and flow rate of 0.8 mL/min (10 MPa). Column temperature was 35 degrees C and operating potentials for electrochemical detection was 0.70 V. To 50 mg brain tissue were 1 mL 50% ammonium sulfate and 4 mL ethyl acetate. The sample was vortexed for 5 min and ultrasonically agitated for 15 min, then centrifuged at 3000 r/min for 15 min. The upper (organic) layer was collected and the lower layer reextracted with 4 mL of ethyl acetate by vigorously vortexing, then centrifuged at 3000 r/min for 15 min. The organic layer was combined with the previously collected ethyl acetate layer. This organic extract was dried under a gentle nitrogen stream, and the residue was reconstituted with 1 mL internal standard of guaifenesinum before HPLC analysis. The linear range was 0.1-10.0 mg/L, and the detection limit 0.1 mg/L. Intra-day and inter-day RSD for assaying brain tissue sample were 0.87% and 1.41%, respectively. The average recovery was 92.87% with coefficient of variation of 2.35%.