HPLC法同时测定丹知青娥片中4种成分的含量
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篇名: HPLC法同时测定丹知青娥片中4种成分的含量
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摘要: 目的:建立同时测定丹知青娥片中补骨脂素、异补骨脂素、补骨脂苷、异补骨脂苷含量的方法。方法:采用高效液相色谱法。色谱柱为Eclipse XDB-C18,流动相分别为甲醇-水(51 ∶ 49,V/V)(等度洗脱分析补骨脂素和异补骨脂素)、乙腈-0.1%甲酸水溶液(12 ∶ 88,V/V)(等度洗脱分析补骨脂苷和异补骨脂苷),流速为1.0 ml/min,检测波长为246 nm,柱温为30 ℃,进样量为10 μl。结果:补骨脂素、异补骨脂素、补骨脂苷和异补骨脂苷的检测质量浓度线性范围分别为3.138~200.8 、3.175~203.2 、3.181~101.8、3.169~101.4 μg/ml(r均为0.999 9);定量限分别为0.627 5、0.635 0、3.181 0、3.169 0 ng,检测限分别为0.251 0、0.254 0、1.273 0、1.268 0 ng;精密度、稳定性、重复性试验的RSD<2%;加样回收率分别为95.68%~102.80%(RSD=2.4%,n=6)、95.91%~102.10%(RSD=2.3%,n=6)、98.64%~99.13%(RSD=0.23%,n=6)、100.20%~101.70%(RSD=0.69%,n=6)。结论:该方法操作简便、结果准确,可用于同时测定丹知青娥片中补骨脂素、异补骨脂素、补骨脂苷、异补骨脂苷的含量。
ABSTRACT: OBJECTIVE: To establish a method for the contents determination of psoralen, isopsoralen, psoralenoside and isopsoralenoside in Danzhi qing’e tablet. METHODS: HPLC performed on the column of Eclipse XDB-C18 with mobile phase of methanol-water (51 ∶ 49,V/V) (isocratic elution, for psoralen and isopsoralen) and acetonitrile-0.1% formic acid (12 ∶ 88,V/V) (isocratic elution, for psoralenoside and isopsoralenoside) at a flow rate of 1.0 ml/min, the detection wavelength was 246 nm, column temperature was 30 ℃, and injection volume was 10 μl. RESULTS: The linear range was 3.138-200.8 μg/ml for psoralen (r=0.999 9), 3.175-203.2 μg/ml for isopsoralen(r=0.999 9),3.181-101.8 μg/ml for psoralenoside (r=0.999 9) and 3.169-101.4 μg/ml for isopsoralenoside (r=0.999 9); RSDs of precision, stability and reproducibility tests were lower than 2%; limits of quantitation were 0.627 5 ng, 0.635 0 ng, 3.181 0 ng and 3.169 0 ng,the limits of detection were 0.251 0 ng, 0.254 0 ng, 1.273 0 ng and 1.268 0 ng; recoveries were 95.68%-102.80%(RSD=2.4%,n=6), 95.91%-102.10%(RSD=2.3%,n=6), 98.64%-99.13%(RSD=0.23%,n=6) and 100.20%-101.70%(RSD=0.69%,n=6), respectively. CONCLUSIONS: The method is simple and accurate, and can be used for the simultaneous determination of psoralen, isopsoralen, psoralenoside and isopsoralenoside in Danzhi qing’e tablet.
期刊: 2016年第27卷第27期
作者: 杨帆,于卉娟,王亚静,杨君君,张波泳,王跃飞,柴欣
AUTHORS: YANG Fan,YU Huijuan,WANG Yajing,YANG Junjun,ZHANG Boyong,WANG Yuefei,CHAI Xin
关键字: 丹知青娥片;含量测定;补骨脂素;异补骨脂素;补骨脂苷;异补骨脂苷; 高效液相色谱法
KEYWORDS: Danzhi qing’e tablet; Content determination; Psoralen; Isopsoralen; Psoralenoside; Isopsoralenoside; HPLC
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