作者首次从天冬样品液制备方法、展开剂筛选、展距确定等方面研究了不同产地的天冬所含有的β-谷甾醇和氨基酸(L-天冬酰胺、精氨酸、亮氨酸、苏氨酸、缬氨酸)的薄层色谱条件。β-谷甾醇的薄层鉴别条件为:用石油醚提取,展开剂为石油醚-醋酸乙酯-甲酸(5:1:0.06),10防硫酸乙醇显色;氨基酸的薄层定性鉴别:无水乙醇冷浸,展开剂为正丁醇-冰醋酸-乙醇-水(4:1:1:2),茚三酮溶液显色;所得出的方法的重现性好,薄层斑点清晰,分离度好,可作为天冬定性鉴别手段之一;有利于天冬CAP研究并为制定天冬药材质量标准提供依据。

OBJECTIVE:To fulfill GAP research,provide scientific basis for establishing quality criteria and study on TLC of Radix Asparagi. METHODS; The authors first study from different aspects,such as the preparation methods of test solutions, the selection of solvent systems and the determination of the developed distance, the TLC conditions of β-sitosterol and amino acids (L-asparagine,arginine,leucine,threonine and valine) contained in Radix Asparagi from different regions. RESULTS: Identification of β-sitosterol: take 4.0g of the powder (through sieve of aperture No. 40)of the sample of Radix Asparagi,extract it by 40ml of petroleum ether(60-90℃ )for 6 hours under reflux, filter it and wash the residues with petroleum ether, evaporate the filtrate to dryness and dissolve the residues in 2ml of petroleum ether as test solution; use n-petroleum ether-ethyl acetate-formic acid (5:l;0.06)as mobile phase,put 50ul of test solution and lul of reference solution on a plate,dry it in the air after developing 8cm and removing the plate,spray with 10% of sulfuric acid in ethanol,heat for 4-5 mins at 105℃ until the appearance of spots obtained by test solution in chromatogram, which correspond in position and color to the spots obtained by reference solution in chromatogram. Identification of amino acids; Macerate Ig of the powder (through sieve of aperture No. 40) of Radix Asparagi in 40ml of absolute ethanol for one night and filter it,evaporate the filtrate to dryness and dissolve the residues in 2ml of ethanol as test solution; use n-butanol-glacial acetic acid-ethanol-water(4; 1; 1 ;2) as mobile phase, put 50ul of test solution and lul of each of reference solutions on a the plate,dry it in the air after developing 14cm and removing the plate,spray with ninhydrin TS evenly and heat at 105℃ until the emergence of spots obtained by test solution in the chromatogram which correspond in position and color to the spots obtained by reference solutions in the chromatogram. CONCLUSION: The TLC identification reported in this paper can provide reproducible results and efficient separations, which can be employed as one of the measurements in the qualitative identification of Radix Asparagi.

四川省科技厅天冬药材内江种植科技示范区项目(2001-11)