摘要
目的:建立一测多评法同时测定马钱子中马钱子碱、士的宁、马钱子碱氮氧化合物、士的宁氮氧化合物4个生物碱的含量。方法:用三氯甲烷对马钱子供试品进行回流提取,提取物采用Agilent ZORBSX Eclipse XDB-C_(18)色谱柱(250 mm×4.6 mm,5μm)进行色谱分析,以乙腈-0.02 mol·L^(-1)磷酸二氢钾溶液(pH 4.0)(23∶77)为流动相,进行等度洗脱,体积流量1.0 mL·min^(-1),柱温35℃,检测波长260 nm。选择士的宁为内标物,计算马钱子及2种氮氧化合物的相对校正因子,分别测定其含量。结果:4个生物碱成分在其浓度范围内线性关系良好(r≥0.9998),平均加样回收率为99.2%~102.3%,RSD为0.72%~1.57%。与外标法比较,测得含量结果无显著性差异(P>0.05)。马钱子碱、士的宁及其氮氧化合物含量测定结果分别为0.746%~1.759%、1.39%~3.27%、0.0165%~0.0561%、0.0352%~0.1190%。结论:建立的方法快捷可靠,尤其适用于马钱子炮制工艺及其炮制品的质量控制。
Objective:To establish a quantitative analysis of multi-components by single-marker(QAMS)method for the simultaneous determination of brucine,strychnine,brucine N-oxide and strychnine N-oxide in Semen Strychni.Methods:The analysis of chloroform reflux extract of Semen Strychni was performed on the Agilent ZORBSX Eclipse XDB-C_(18) column(250 mm×4.6 mm,5μm),with the mobile phase consisted of acetonitrile-0.02 mol·L^(-1) potassium dihydrogen phosphate solution(pH 4)(23∶77).The flow rate was 1.0 mL·min^(-1).The column temperature was 35℃and the detection wavelength was 260 nm.Strychnine was used as the internal standard.The relative correction factors of strychnine and the N-oxides were calculated,and the contents of the four components were measured separately.Results:Four constituents showed good linear relationship within their own ranges(r≥0.9998),whose average recoveries were 99.2%-102.3%with RSDs of 0.72%-1.57%.The results obtained by QAMS showed no significant difference compared to the external standard method(EMS)(P>0.05).The contents of brucine,strychnine and their N-oxides were 0.746%-1.759%,1.39%-3.27%,0.0165%-0.0561%,and 0.0352%-0.1190%,respectively.Conclusion:The method is simple,fast,accurate and reliable,and it’s especially suitable for the quality control of the processing technology and processed products of Semen Strychni.
作者
杜鑫
唐丽婧
谈利红
贾清树
李艳
DU Xin;TANG Li-jing;TAN Li-hong;JIA Qing-shu;LI Yan(Chongqing Medical and Pharmaceutical College,Chongqing Key Laboratory of High Active Traditional Chinese Drug Delivery System,Chongqing 401331,China;The People’s Hospital of Tongliang District,Chongqing City,Chongqing 402560,China;Taiji Group Sichuan Mianyang Pharmaceutical Co.,Ltd.,Mianyang 621000,China)
出处
《药物分析杂志》
北大核心
2025年第4期564-570,共7页
Chinese Journal of Pharmaceutical Analysis
基金
重庆市自然科学基金面上项目(cstc2021jcyj-msxmX0452)
重庆市沙坪坝区科卫联合医学科研项目(2023SQKWLH039)
重庆医药高等专科学校科研项目(ygzzd2024101)。
