天然产物研究与开发 ›› 2021, Vol. 33 ›› Issue (9): 1572-1581.doi: 10.16333/j.1001-6880.2021.9.015

• 开发研究 • 上一篇    下一篇

TLC-NIRS联用技术快速检测保健品中非法添加性保健类化学药物研究

张立军1,贾建忠3,张新玥2,张转平1*,谭华森1,徐桂新1,李小安1,刘家佳1   

  1. 1陕西省安康市食品药品检验检测中心,安康 725000;2北京中医药大学 中药学院,北京 100029;3陕西省食品药品研究院,西安 710061
  • 出版日期:2021-09-28 发布日期:2021-09-28
  • 基金资助:
    陕西省社会发展科技攻关项目(2015SF286)

Determination of sex-enhancing drugs illegally added in health care products by TLC-NIRS combined technology

ZHANG Li-jun1,JIA Jian-zhong3,ZHANG Xin-yue2,ZHANG Zhuan-ping1*,TAN Hua-sen1,XU Gui-xin1,LI Xiao-an1,LIU Jia-jia1#br#

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  1. 1 Ankang Inspection and Detection Center of Food and Drug Control,Ankang 725000,China;2 Department of Chinese Medicine,Beijing University of Chinese Medicine,Beijing 100029,China;3 Shanxi Institute for Food and Drug Control,Xi'an 710061,China

  • Online:2021-09-28 Published:2021-09-28

摘要:

建立保健品中非法添加性保健类化学药物薄层色谱(TLC)-近红外光谱(NIRS)检测模型,用于保健品中添加违禁化学药物快速定性定量分析。采用高效液相色谱(HPLC)建立违禁化学药物含量测定法,作为参考值。采用TLC法,以三氯甲烷-甲醇-氨水(10∶1∶0.1)为添加违禁化学药物的展开剂,紫外灯下检视标记,利用NIRS仪分别采集TLC上化学药物斑点的NIRS,采用偏最小二乘法(PLS)结合交叉验证法分别建立化学药物最优定性定量分析模型,并进行模型验证。所建立的HPLC含量测定方法分离度好、线性范围宽、准确度高。建立的西地那非、那红地那非TLC-NIRS快速定性定量检测模型经方法学验证线性范围宽、专属性强、模型稳定性好、预测结果好。建立的西地那非、那红地那非TLC-NIRS定量分析模型的决定系数(R2)、验证均方差(RMSECV)、预测均方差(RMSEP)分别为0.984、0.085、0.081和0.982、0.098、0.087。应用TLC-NIRS模型在10批性保健品中检测出9批添加了西地那非,检出率90%;西地那非、那红地那非含量预测值的平均相对偏差分别为1.86%、1.96%。结果表明,建立TLC-NIRS定性定量分析模型通用性强、操作简便,可用于市场上保健品中非法添加上述性保健类化学药物快速检测,为保健品非法添加快速检测研究提供科学思路。

关键词: 保健品, 非法添加, 薄层色谱-近红外光谱联用技术, 高效液相色谱, 性保健

Abstract:

To establish the detection model of sex-enhancing drugs illegally added by the thin layer chromatography (TLC) and near-infrared spectroscopy (NIRS) combined technology,for the rapid qualitative and quantitative analysis of drugs illegally added in health care products.With the content of chemical drugs in health care products determined by HPLC method as a reference value.TLC was used in the study.Trichloromethane-methyl alcohol-ammonium hydroxide (10∶1∶0.1) was used as developing solvent and the plate was detected under ultraviolet lamp.The NIR spectrum of chemical component spots on TLC were collected by NIRS.The rapid qualitative and quantitative model of chemical drugs was established by using the partial least squares regression analysis (PLS) combined with cross validation method.And validated for model.Established the HPLC analysis method with better separation degree and wide linear range.Established the TLC-NIRS analysis models of sildenafil and noracetildenafil with wide linear range,and the better stable and predicted results.The correlation coefficient (R2),the root mean square error of calibration validation (RMSECV) and the root mean square error of prediction (RMSEP) were 0.984,0.085 and 0.081;0.982,0.098 and 0.087,respectively.Using the TLC-NIRS model,9 batches of in 10 batches of sex-enhancing products were detected to be added sildenafil and an unqualified rate of 90%,the average relative 〖JP3〗deviation of the content of sildenafil and noracetildenafil of predicted were 1.86%,1.96%,respectively.The results showed that the TLC-NIRS analysis models can be used for above chemical components rapid determination in sex-enhancing products.The method with specific and simple.Which provided the ideas for rapid determination of added illegally drugs in health care products.

Key words: health care products, added illegally, TLC-NIRS, HPLC, sex-enhancing product

中图分类号:  R917 R979.2