天然产物研究与开发 ›› 2022, Vol. 34 ›› Issue (5): 856-863.doi: 10.16333/j.1001-6880.2022.5.015

• 开发研究 • 上一篇    下一篇

红外光谱结合化学计量学快速检测熊胆粉真伪及掺伪问题

袁明昊1,周   涛1,钟文潇1,周   强1,雷苛露1,曾大富2,李建刚2,郭   力1*   

  1. 1成都中医药大学药学院西南特色中药资源国家重点实验室;2成都晶博生物科技有限责任公司,成都 611137
  • 出版日期:2022-05-28 发布日期:2022-05-23
  • 基金资助:
    四川省科技基础条件平台项目(2019JDPT0032);“杏林学者”学科人才科研提升计划(CXTD2018012)

Rapid detection of authenticity and adulteration of bear bile powder by FTIR spectroscopy combined with chemometrics

YUAN Ming-hao1,ZHOU Tao1,ZHONG Wen-xiao1,ZHOU Qiang1,LEI Ke-lu1,ZENG Da-fu2,LI Jian-gang2,GUO Li1*   

  1. 1State Key Laboratory of Southwestern Chinese Medicine Resources,School of Pharmacy,Chengdu University of Traditional Chinese Medicine;2Chengdu Jingbo Biotechnology Co.,Ltd.,Chengdu 611137,China
  • Online:2022-05-28 Published:2022-05-23

摘要:

利用红外光谱技术对熊胆粉正品、伪品及掺伪品进行快速鉴别并预测掺伪比例,建立熊胆粉的快速质量评价方法。采集94批熊胆粉正品、70批伪品(猪胆粉、牛胆粉、羊胆粉、兔胆粉、鸡胆粉、鸭胆粉、鹅胆粉)及180批掺伪品(掺伪猪胆粉、掺伪牛胆粉)的红外光谱图,利用正交偏最小二乘判别分析(OPLS-DA)及偏最小二乘回归(PLSR)分别建立熊胆粉正品、伪品和掺伪品的定性校正模型及不同类别掺伪品掺伪比例的定量校正模型。熊胆粉正品、伪品及掺伪品的定性校正模型对样本的判别准确率分别为99.64%(校正集)和95.65%(验证集);通过进一步判别分析,可鉴别熊胆粉伪品及掺伪品种类,准确率均大于95%;在2个不同类别掺伪品定量校正模型中,验证集相关系数(R2V)和预测均方根误差(RMSEP)分别为0.987 4、2.630 0%(熊胆粉掺伪猪胆粉)和0.982 6、3.188 7%(熊胆粉掺伪牛胆粉);3个定性模型及2个定量模型均表现出优秀的预测能力。本研究建立的红外光谱结合化学计量学方法可实现对熊胆粉正品、伪品和掺伪品的快速鉴别及掺伪比例确定,为熊胆粉的质量控制及评价提供参考。

关键词: 红外光谱, 熊胆粉, 真伪, 掺伪, 正交偏最小二乘判别分析, 偏最小二乘回归

Abstract:

To establish a rapid quality evaluation method of bear bile powder,infrared spectroscopy was introduced to distinguish bear bile powder from its counterfeits and adulterants.In addition,the adulterated proportion was predicted by infrared spectroscopy combined with chemometrics.Infrared spectra of 94 batches of bear bile powder,70 batches of its counterfeits (pig bile powder,cow bile powder,goat bile powder,rabbit bile powder,chicken bile powder,duck bile powder and goose bile powder) and 180 batches of its adulterants (bear bile powder adulterated with pig bile powder,bear bile powder adulterated with cow bile powder) were collected.Orthogonal partial least squares discriminant analysis (OPLS-DA) was used to establish the qualitative correction models of bear bile powder,its counterfeits and adulterants.Partial least squares regression (PLSR) was used to establish the quantitative correction models of adulterated proportions of different kinds of adulterants.The accuracy of the qualitative correction model for bear bile powder,its counterfeits and adulterants was 99.64% (calibration set) and 95.65% (verification set),respectively.According to further discriminant analysis,the category of the counterfeit and adulterated bear bile powder could be identified with an accuracy greater than 95%.In the two quantitative correction models,the correlation coefficients of the validation set (R2V) and the root mean square error of prediction (RMSEP) were 0.987 4,2.630 0% (bear bile powder adulterated with pig bile powder) and 0.982 6,3.188 7% (bear bile powder adulterated with cow bile powder),respectively.The three qualitative models and two quantitative models all showed excellent predictive ability.The method of infrared spectroscopy combined with chemometrics established in this study can realize the rapid identification of bear bile powder,its counterfeits and adulterants as well as the determination of adulterated proportion.It also provides a meaningful reference for quality control and evaluation of bear bile powder.

Key words: infrared spectroscopy, bear bile powder, authenticity, adulteration, orthogonal partial least squares discriminant analysis (OPLS-DA), partial least squares regression (PLSR)

中图分类号:  R284.1