摘要
目的 提升接骨丹片的质量标准。方法 采用薄层色谱法鉴别制剂中的制马钱子和大黄;采用高效液相色谱法同时测定马钱子碱和士的宁的含量,色谱柱为Kromasil 100-5-C_(18)柱(250 mm×4.6 cm,5μm),流动相为乙腈-0.01 mol/L庚烷磺酸钠与0.02 mol/L磷酸二氢钾等量混合溶液进行梯度洗脱,流速为1.0 mL/min,检测波长为260 nm,柱温为30℃,进样量为10μL。结果 制马钱子、大黄的薄层色谱图斑点清晰,分离度高,且阴性对照无干扰。马钱子碱和士的宁的质量浓度分别在1.46~116.73μg/mL和1.60~128.30μg/mL范围内与峰面积线性关系良好(r=0.999 5,0.999 7,n=6);精密度、重复性、稳定性试验结果的RSD均小于2.0%(n=6);平均加样回收率分别为97.28%和96.23%,RSD分别为1.16%和1.36%(n=6)。结论 该方法专属性好,结果准确、可靠,可用于接骨丹片的质量评价。
Objective To improve the quality standard of Jiegudan Tablets.Methods Processed Strychnine Semen and Rhei Radix et Rhizoma in the preparation were qualitatively identified by the thin-layer chromatography(TLC)method.The contents of brucine and strychnine in the preparation were determined by the high-performance liquid chromatography(HPLC)method,the chromatographic column was Kromasil 100-5-C_(18) column(250 mm×4.6 mm,5μm),the mobile phase was mixed solution of the equal amount of acetonitrile-0.01 mol/L sodium heptanesulfonate and 0.02 mol/L potassium dihydrogen phosphate(gradient elution),the flow rate was 1.0 mL/min,the detection wavelength was 260 nm,the column temperature was 30℃,and the injection volume was 10μL.Results The TLC chromatograms of processed Strychnine Semen and Rhei Radix et Rhizoma showed clear spots and good separation,with no interference from the negative reference.The linear ranges of brucine and strychnine were 1.46-116.73μg/mL and 1.60-128.30μg/mL(r=0.9995,0.9997,n=6),respectively.The RSDs of precision,repeatability and stability test results were lower than 2.0%(n=6).The average recoveries of brucine and strychnine were 97.28%and 96.23%,with RSDs of 1.16%and 1.36%(n=6),respectively.Conclusion The established method is accurate and reliable,which can be used for the quality evaluation of Jiegudan Tablets.
作者
蔡秀娟
林向前
林石明
CAI Xiujuan;LIN Xiangqian;LIN Shiming(Zhangzhou Hospital of Traditional Chinese Medicine,Zhangzhou,Fujian,China 363000)
出处
《中国药业》
CAS
2024年第1期87-90,共4页
China Pharmaceuticals
基金
福建省漳州市卫生健康委员会2023-2026年度市中医药科研课题[2023ZY01]。
