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-C18色谱柱（250 mm×4.6 mm,5 μm）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≥0.999 8）,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%、0.016 5%~0.056 1%、0.035 2%~0.119 0%。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-C18 column (250 mm×4.6 mm, 5 μm), 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 was35 ℃ 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≥0.999 8), 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%, 0.016 5%-0.056 1%, and 0.035 2%-0.119 0%,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.
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