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作 者:敖敦格日乐[1,2] 拉喜那木吉拉 吴香杰 Aodungerile;Laxinamujila;WU Xiangjie(Mongolian Medical College,Inner Mongolia Minzu University,Tongliao,Inner Mongolia,China 028000;NMPA Key Laboratory for Quality Control of Traditional Chinese Medicine
机构地区:[1]内蒙古民族大学蒙医药学院,内蒙古通辽028000 [2]国家药监局中药<蒙药>质量控制重点实验室,内蒙古通辽028000
出 处:《中国药业》2022年第17期61-64,共4页China Pharmaceuticals
基 金:内蒙古自治区科技计划项目[2021GG0002];内蒙古蒙医药工程技术研究院科研课题[GCY201508013];2021年“草原英才”人才项目[CYYC21003];内蒙古民族大学自然科学一般项目[NMDYB19073]。
摘 要:目的 建立蒙药杠柳的质量标准。方法 采用薄层色谱法定性鉴别槲皮素和山柰素;采用高效液相色谱法测定4-甲氧基水杨醛和槲皮素的含量,色谱柱为Promosil C柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.1%磷酸溶液(45∶55,V/V),流速为1.0 mL/min,检测波长为360 nm,柱温为32℃,进样量为10μL。结果 薄层色谱鉴别中,供试品溶液在3种展开系统[正己烷-乙酸乙酯-甲酸(9∶6∶1,V/V/V)、三氯甲烷-乙酸乙酯-甲酸(6∶4∶1,V/V/V)、环己烷-乙酸乙酯-甲酸(6∶5∶1,V/V/V)]下均检出槲皮素和山柰素特征斑点。4-甲氧基水杨醛和槲皮素的进样量分别在0.277 0~1.662 0μg(r=0.999 8,n=6)和0.082 5~0.495 0μg(r=0.999 7,n=6)范围内与峰面积线性关系良好;精密度、稳定性、重复性试验的RSD均小于2.0%(n=6);平均加样回收率分别为96.78%和102.05%,RSD分别为5.38%和2.78%(n=18)。药材样品中4-甲氧基水杨醛和槲皮素的含量分别为2.35~6.68 mg/g和0.28~2.09 mg/g。结论 该方法操作简便、结果准确、稳定性和重复性均较好,可用于蒙药杠柳的质量控制。Objective To establish the quality standard of Mongolian medicine Periploca sepium.MethodsQuercetin and kaempferol were qualitatively identified by the thin-layer chromatography (TLC) method.The contents of 4-mthoxysalicylaldehyde and quercetin were determined by the high-performance liquid chromatography (HPLC) method.The chromatographic column was Promosil Ccolumn (250 mm×4.6 mm,5μm),the mobile phase was methanol-0.1%phosphoric acid solution (45∶55,V/V),the flow rate was 1.0 mL/min,the detection wavelength was 360 nm,the column temperature was 32℃,and the injection volume was 10μL.ResultsThe TLC chromatograms showed that the characteristic spots of quercetin and kaempferol were detected in the test solution with the three development systems including n-hexane-ethyl acetate-formic acid (9∶6∶1,V/V/V),chloroformethyl acetate-formic acid (6∶4∶1,V/V/V) and cyclohexane-ethyl acetate-formic acid (6∶5∶1,V/V/V).The linear ranges of 4-mthoxysalicylaldehyde and quercetin were 0.277 0-1.662 0μg(r=0.999 8,n=6)and 0.082 5-0.495 0μg(r=0.999 7,n=6),respectively.The RSDs of precision,stability and repeatability tests were lower than 2.0%(n=6).The average recoveries of4-mthoxysalicylaldehyde and quercetin were 96.78%and 102.05%with RSDs of 5.38%and 2.78%(n=18),respectively.The contents of 4-mthoxysalicylaldehyde and quercetin in the samples were in the range of 2.35-6.68 mg/g and 0.28-2.09 mg/g,respectively.ConclusionThe method is simple,accurate,stable and repeatable,which can be used for the quality control of Mongolian medicine Periploca sepium.
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