高效液相色谱法测定红景天提取物中红景天苷的不确定度评定

Uncertainty evaluation for determination of salidroside in Rhodiola rosea L. extract by high performance liquid chromatography

中文关键词:  红景天  红景天苷  不确定度  高效液相色谱法

英文关键词:Rhodiola rosea L.  salidroside  uncertainty  high performance liquid chromatography

中文摘要:

      目的 评定高效液相色谱法测定红景天提取物中红景天苷含量的不确定度。方法 根据JJF 1059.1-2012《测量不确定度评定与表示》, 用甲醇提取样品中的红景天苷, 在波长275 nm下, 用紫外检测器进行测定。通过分析影响不确定度因素的来源, 对不确定度进行量化分析, 从而得出扩展不确定度。结果 当置信水平为95%, 包含因子k=2时, 其扩展不确定度为±0.17 g/100 g, 红景天提取物中红景天苷含量为(4.03±0.17) g/100 g。不确定度主要来源于标准曲线拟合、测量重复性和标准溶液配制。结论 高效液相色谱仪应定期进行校准与维护保养, 定期检查紫外灯能量和自动进样器的定量准确性, 选用高校准级别的容量瓶、高纯度的标准品。检测人员应熟练掌握样品的各项处理步骤, 以提高检测准确性。

英文摘要:

      Objective To evaluate the uncertainty for the determination of salidroside in Rhodiola rosea L. extract by high performance liquid chromatography (HPLC). Methods According to JJF 1059.1-2012 Evaluation and expression of measurement uncertainty, salidroside was extracted with methanol, the determination was carried out with ultravioletray (UV) detector at 275 nm. Through the analysis of the sources of influencing factors in uncertainty, the uncertainty was quantitatively analyzed to obtain the expanded uncertainty. Results The expanded uncertainty was ±0.17 g/100 g when the confidence level was 95% and influencing factor was 2. The salidroside content in Rhodiola rosea L. extract was (4.03±0.17) g/100 g. The main sources of uncertainty were calibration curve fitting, repeatability of measurement and preparation of standard solution. Conclusion We should regularly calibrate and maintain the high performance liquid chromatography, regularly check the energy of UV lamp and the quantitative accuracy of automatic injector, and use the capacity bottle of high level and high purity standard. The experimenter should be skilled with the sample processing steps to improve the detection accuracy.