法医学杂志

法医学杂志 ›› 2021, Vol. 37 ›› Issue (1): 33-37.DOI: 10.12116/j.issn.1004-5619.2019.390901

• 论 著 • 上一篇    下一篇

红外光谱法用于安钠咖中咖啡因和苯甲酸钠快速定性和定量分析

苏承轲1 ，刘翠梅2 ，孟鑫2 ，花镇东2 ，段凯1   

  1. 1. 鄂尔多斯市公安局，内蒙古 鄂尔多斯 017000；2. 公安部禁毒情报技术中心 毒品监测管控与禁毒关键 技术公安部重点实验室，北京 100193
  • 收稿日期:2019-09-17 发布日期:2021-02-25 出版日期:2021-02-28
  • 通讯作者: 刘翠梅，女，博士，副研究员，主要从事毒品鉴定与特征分析研究；E-mail：liucuimei8258@163.com
  • 作者简介:苏承轲（1991—），男，硕士，主要从事毒品检验鉴定；E-mail：617976875@qq.com
  • 基金资助:
    国家重点研发计划资助项目（2016YFC0800903）

Rapid Qualitative and Quantitative Analysis of Caffeine and Sodium Benzoate in Annaca by Infrared Spectroscopy

SU Cheng-ke1 , LIU Cui-mei2 , MENG Xin2 , HUA Zhen-dong2 , DUAN Kai1   

  1. 1. Ordos Public Security Bureau, Ordos 017000, Inner Mongolia Autonomous Region, China; 2. Key Labora? tory of Drug Monitoring and Control, Drug Intelligence and Forensic Center, the Ministry of Public Securi? ty of the People’s Republic of China, Beijing 100193, China
  • Received:2019-09-17 Online:2021-02-25 Published:2021-02-28

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摘要： 目的 建立安钠咖样品中咖啡因和苯甲酸钠快速定性和定量分析的红外光谱方法。 方法 采用 高纯度咖啡因和苯甲酸钠混合制样的方法制备定性和定量建模样品，通过分析混合样品的红外光谱图， 确定安钠咖样品中咖啡因和苯甲酸钠的特征吸收峰。采用偏最小二乘法（partial least squares，PLS）建立 红外光谱定量模型。 结果 通过分析17个咖啡因和苯甲酸钠混合样品（咖啡因纯度范围10%~80%）的红 外光谱图，确定了咖啡因的特征吸收峰为1 698、1 650、1 237、972、743、609 cm-1 ；苯甲酸钠的特征吸收峰为 1 596、1 548、1 406、845、708、679 cm-1 。将所有特征吸收峰均检出作为阳性判断依据时，48个安钠咖缴获样 品中咖啡因和苯甲酸钠的阳性检出率均为100%。咖啡因PLS定量模型的线性范围为10%~80%，决定系数 （R2 ）为 99.9%，交叉验证均方差（root mean square error of cross validation，RMSECV）为 0.68%，预测均方 差（root mean square error of prediction，RMSEP）为 0.91%；苯甲酸钠 PLS 定量模型的线性范围为 20%~ 90%，R2 为99.9%，RMSECV为0.91%，RMSEP为1.11%。配对样本t检验结果显示，高效液相色谱法和红外 光谱法的测定结果差异无统计学意义。采用所建立的红外定量方法分析48个安钠咖缴获样品，咖啡因的 纯度为27.6%~63.1%，苯甲酸钠的纯度为36.9%~72.3%。 结论 采用红外光谱法对安钠咖样品中的咖啡因 和苯甲酸钠进行快速定性和定量分析，可提高检验鉴定效率、降低检验成本。

关键词: 法医毒理学；谱学, 傅里叶变换红外；安钠咖；咖啡因；苯甲酸钠

Abstract: Objective To establish an infrared spectroscopic method for the rapid qualitative and quantitative analysis of caffeine and sodium benzoate in Annaka samples. Methods Qualitative and quantitative modeling samples were prepared by mixing high-purity caffeine and sodium benzoate. The characteristic absorption peaks of caffeine and sodium benzoate in Annaka samples were determined by analyzing the infrared spectra of the mixed samples. The quantitative model of infrared spectra was established by partial least squares （PLS）. Results By analyzing the infrared spectra of 17 mixed samples of caffeine and sodium benzoate （the purity of caffeine ranges from 10% to 80%）, the characteristic absorption peaks for caffeine were determined to be 1 698, 1 650, 1 237, 972, 743, and 609 cm- 1 . The characteristic absorption peaks for sodium benzoate were 1 596, 1 548, 1 406, 845, 708 and 679 cm- 1 . When the detection of all characteristic absorption peaks was the positive identification criteria, the positive detection rate of caffeine and sodium benzoate in 48 seized Annaka samples was 100%. The linear range of PLS quantitative model for caffeine was 10%-80%, the coefficient of determination （R2 ） was 99.9% , the root mean square error of cross validation （RMSECV） was 0.68% , and the root mean square error of prediction （RMSEP） was 0.91%; the linear range of PLS quantitative model for sodium benzoate was 20%-90% , the R2 was 99.9% , the RMSECV was 0.91% and the RMSEP was 1.11% . The results of paired sample t test showed that the differences between the results of high performance liquid chromatography method and infrared spectroscopy method had no statistical significance. The established infrared quantitative method was used to analyze 48 seized Annaka samples, the purity of caffeine was 27.6%-63.1%, and that of sodium benzoate was 36.9%-72.3%. Conclusion The rapid qualitative and quantitative analysis of caffeine and sodium benzoate in Annaka samples by infrared spectroscopy method could improve identification efficiency and reduce determination cost.

Key words: forensic toxicology, spectroscopy, Fourier transform infrared, Annaka, caffeine, sodium benzoate

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