中药复方莲松异搏停片的定性定量方法研究

目的：建立中药莲松异搏停片的定性定量方法。 方法：采用薄层色谱法对炙甘草、丹参、莲子心、延胡索、苦参进行定性鉴别。炙甘草TLC条件：1%氢氧化钠溶液制备的硅胶G薄层板，三氯甲烷-甲醇-水（13：7：2）的下层溶液为展开剂；丹参TLC条件：硅胶GF₂₅₄薄层板，甲苯-三氯甲烷-乙酸乙酯-甲醇-甲酸（2：3：4：0.5：2）为展开剂；莲子心TLC条件：硅胶G薄层板，三氯甲烷-乙酸乙酯-二乙胺（1：6：1）为展开剂；延胡索TLC条件：硅胶G薄层板，环己烷-乙醚-甲醇（3：5：0.5）为展开剂；苦参TLC条件：硅胶G薄层板上，以三氯甲烷-甲醇-氨水（25：1：1）的下层溶液为展开剂。采用高效液相色谱法对炙甘草中甘草酸进行含量测定。HPLC条件：采用Welch Ultimate XB-C₁₈色谱柱（4.6 mm×250 mm，5 μm），流动相为甲醇-磷酸二氢铵溶液（取磷酸二氢铵1.725 g，加水300 mL溶解，用磷酸调节pH至3.5）（61：39），流速1.0 mL·min^-1，检测波长251 nm。 结果：定性鉴别斑点清晰，方法稳定可靠；甘草酸在0.19~4.76 μg范围内呈良好的线性关系（r=0.9999），平均回收率（n=9） 为100.2%。 结论：本制剂质量标准所建立方法专属性好，灵敏度高，可用于莲松异搏停片的质量控制。

Objective: To establish the qualitative and quantitative methods of Liansong Yiboting tablets. Methods: Glycyrrhizae Radix et Rhizoma Praeparata Cum Melle,Salviae Miltiorrhizae Radix et Rhizoma,Nelumbinis Plumula,Corydalis Rhizoma and Sophorae Flavescentis Radix were identified by TLC.TLC condition of Glycyrrhizae Radix et Rhizoma Praeparata Cum Melle:using silica gel G mixed with sodium carboxymethyl cellulose containing 1% sodium hydroxide as the coating substance and the lower solution of chloroform-methanol-water(13: 7: 2) as the mobile phase;TLC condition of Salviae Miltiorrhizae Radix et Rhizoma:using silica gel GF₂₅₄ as the coating substance and toluene-chloroform-ethyl acetate-methanol-formic acid(2: 3: 4: 0.5: 2)as the mobile phase;TLC condition of Nelumbinis Plumula:using silica gel G as the coating substance and chloroform-ethyl acetate-diethylamine(1: 6: 1) as the mobile phase;TLC condition of Corydalis Rhizoma:using silica gel G as the coating substance and cyclohexane-ethyl ether-methanol(3: 5: 0.5) as the mobile phase;TLC condition of Sophorae Flavescentis Radix:using silica gel G as the coating substance and the lower solution of chloroform-methanol-ammonia(25: 1: 1) as the mobile phase.HPLC conditions of glycyrrhizic acid:using Welch Ultimate XB-C₁₈(4.6 mm×250 mm,5 μm) column as analytic column and methanol-solution of ammonium dihydrogen phosphate(the solution of ammonium dihydrogen phosphate:accurately weigh 1.725 g of ammonium dihydrogen phosphate,add 300 mL of water to dissolve it,adjusted to pH 3.5 with phosphoric acid) (61: 39) as the mobile phase,with a flow rate of 1.0 mL·m in^-1 and UV detection at 251 nm. Results: Identification spots were clear,and this method was stable and reliable.The glycyrrhizic acid showed good linear relationship (r=0.9999) in the range of 0.19-4.76 μg.The average recovery(n=9) was 100.2%. Conclusion: This method has a strong specificity,high sensitivity and can be used for quality control of the Liansong Yiboting tablets.