摘要
目的 提升春生丸的质量标准。方法 对制剂中的枸杞子、黄芪、黄芩进行显微鉴别;采用薄层色谱(TLC)法对制剂中的菟丝子、何首乌、淫羊藿进行定性鉴别;采用超高效液相色谱(UPLC)法测定制剂中王不留行黄酮苷、2,3,5,4'-四羟基二苯乙烯-2-O-β-D-葡萄糖苷、金丝桃苷、黄芩苷的含量,色谱柱为Acquity UPLC BEH C18柱(100 mm×2.1 mm,1.8μm),流动相为甲醇-0.2%磷酸水溶液(梯度洗脱),流速为0.3 mL/min,检测波长分别为280 nm(黄芩苷)、320 nm(王不留行黄酮苷、2,3,5,4'-四羟基二苯乙烯-2-O-β-D-葡萄糖苷)、360 nm(金丝桃苷),进样量为2μL。结果 枸杞子、黄芪、黄芩显微特征明显。菟丝子、何首乌、淫羊藿的TLC图斑点清晰,分离度好,阴性对照无干扰。王不留行黄酮苷、2,3,5,4'-四羟基二苯乙烯-2-O-β-D-葡萄糖苷、金丝桃苷、黄芩苷质量浓度分别在0.008~0.032 mg/mL、0.074~0.296 mg/mL、0.015~0.060 mg/mL、0.263~1.054 mg/mL范围内与峰面积线性关系良好(r> 0.999 0);精密度、稳定性、重复性试验结果的RSD均小于2.0%;平均加样回收率分别为100.87%,100.43%,98.43%,98.78%,RSD分别为1.66%,2.44%,2.08%,1.49%(n=6)。结论 所建方法操作简便,可用于春生丸的质量控制。
Objective To improve the quality standard of Chunsheng Pills.Methods Lycii Fructus,Astragali Radix and Scutellariae Radix in the preparation were identified by the microscope.Cuscutae Semen,Polygoni Multiflori Radix,Epimedii Folium in the preparation were identified qualitatively by the thin-layer chromatography(TLC)method.The flavonoids in Vaccariae Semen,2,3,5,4'-tetrahydroxystilbene-2-O-β-D-glucoside,hyperoside and baicalin contents in the preparation were determined by the ultra-high-performance liquid chromatography(UPLC)method;the chromatographic column was the Acquity UPLC BEH C18 column(100 mm×2.1 mm,1.8μm),the mobile phase was methanol-0.2%phosphoric acid aqueous solution(gradient elution),the flow rate was 0.3 mL/min,and the detection wavelengths were 280 nm(baicalin),320 nm(flavonoids in Vaccariae Semen,2,3,5,4'-tetrahydroxystilbene-2-O-β-D-glucoside),360 nm(hyperoside),and the injection volume was 2μL.Results The microscopic characteristics of Lycii Fructus,Astragali Radix and Scutellariae Radix were obvious.The TLC chromatograms of Cuscutae Semen,Polygoni Multiflori Radix,Epimedii Folium had clear spots,good resolution,and there was no interference from the negative reference.The linear ranges of flavonoids in Vaccariae Semen,2,3,5,4'-tetrahydroxystilbene-2-O-β-D-glucoside,hyperoside and baicalin were 0.008-0.032 mg/mL,0.074-0.296 mg/mL,0.015-0.060 mg/mL,0.263-1.054 mg/mL,respectively(r>0.9990).The RSDs of precision,stability and repeatability tests were all lower than 2.0%.The average recovery rates of flavonoids in Vaccariae Semen,2,3,5,4'-tetrahydroxystilbene-2-O-β-D-glucoside,hyperoside and baicalin were 100.87%,100.43%,98.43%,98.78%,with RSDs of 1.66%,2.44%,2.08%,1.49%respectively(n=6).Conclusion The established method is easy,which can be used for the quality control of Chunsheng Pills.
作者
宿曼筠
傅超
杨晓云
王友兰
卢京光
SU Manyun;FU Chao;YANG Xiaoyun;WANG Youlan;LU Jingguang(Qingdao Research Institute for Food and Drug Control·NMPA Key Laboratory for Quality Research and Evaluation of Traditional Marine Chinese Medicine,Qingdao,Shandong,China 266071)
出处
《中国药业》
CAS
2024年第18期78-82,共5页
China Pharmaceuticals
基金
中国药品监管科学行动计划第二批重点项目[NMPAJGKX-2023-061
NMPAJGKX-2023-0062]。
