基于不确定曲线策略的近红外定量分析丹参酮提取物中丹参酮ⅡA含量  

Determination of tanshinoneⅡA content in tanshinone extract by near infrared spectroscopy based on uncertainty profile strategy

作　　者：薛忠[1] 刘德玄 曹春琪 徐冰[3,4] 王亚博 律涛[1] XUE Zhong;LIU De-xuan;CAO Chun-qi;XU Bing;WANG Ya-bo;LU Tao(School of Pharmacy,Hebei Medical University,Shijiazhuang 050017,China;Hebei Institute for Drug and Medical Device Control,Shijiazhuang 050200,China;Department of Information of Traditional Chinese Medicine,Beijing University of Chinese Medicine,Beijing 102400,China;Beijing Key Laboratory for Production Process Control and Quality Evaluation of Traditional Chinese Medicine,Beijing Municipal Science&Technology Commission,Beijing 102400,China)

机构地区：[1]河北医科大学药学院,石家庄050017 [2]河北省药品医疗器械检验研究院,石家庄050200 [3]北京中医药大学中药信息学系,北京102400 [4]北京市科委中药生产过程控制与质量评价北京市重点实验室,北京102400

出　　处：《药物分析杂志》2023年第12期2147-2153,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：河北省自然科学基金(H2021206101)。

摘　　要：目的:基于不确定度曲线建立丹参酮提取物中丹参酮ⅡA含量的近红外(NIR)定量分析方法。方法:采集丹参酮提取物近红外光谱,采用HPLC作为参考方法分析丹参酮提取物中丹参酮ⅡA的含量,建立丹参酮提取物中ⅡA含量和近红外光谱之间的偏最小二乘(PLS)定量模型。通过K-S(Kennard-Stone)方法划分校正集和校正测试集,比较不同的光谱预处理方法建立最优PLS定量回归模型。采用“6×3×3”验证实验得到验证数据,得出NIR分析方法的验证信息,并计算NIR定量分析方法的不确定度,构建不确定度曲线并评价所建立方法的有效性。结果:选择1std数据预处理方法来建立PLS定量回归模型,所建立的NIR定量分析方法真实性,精密度良好,丹参酮ⅡA含量的有效定量范围为2.04%~27.64%,分析结果准确有效。结论:不确定曲线策略可以同时提供NIR分析方法的验证信息和不确定度信息,能够降低分析方法的使用风险,保障NIR分析结果的准确性和可靠性。Objective:To establish a near infrared(NIR)quantitative analysis method for testing tanshinoneⅡA content in tanshinone extract based on uncertainty profile.Methods:The near-infrared spectrum of tanshinone extract was collected,and the content of tanshinoneⅡA in tanshinone extract was analyzed by HPLC as a reference method.Partial least squares(PLS)quantitative model between the content of tanshinoneⅡA in tanshinone extract and the near-infrared spectrum was established.The calibration set and calibration test set were divided by K-S(Kennard-Stone)method,and the optimal PLS quantitative regression model was established by comparing different spectral pretreatment methods.The validation information of the NIR analysis method was obtained by the“6×3×3”validation experiments,the uncertainty of the NIR quantitative analysis method was calculated,the uncertainty profile was constructed to evaluate the effectiveness of the NIR method.Results:The quantitative regression model of PLS was established after the 1std data pretreatment method.The trueness and precision of the established NIR quantitative analysis method was good.The effective quantitative range of tanshinoneⅡA content was 2.04%-27.64%,and the analysis results were accurate and effective.Conclusion:The uncertainty profile strategy can provide the validation information and uncertainty information of NIR analysis method at the same time,reduce the risk of using the analysis method,and ensure the accuracy and reliability of NIR analysis results.

关 键 词：不确定度曲线 方法验证 不确定度测量 近红外 丹参酮 丹参酮ⅡA 

分 类 号：R917[医药卫生—药物分析学]