Identification of Alumen and Ammonium alum Based on XRD， FTIR， TG-DTA Combined with Chemometrics
10.13422/j.cnki.syfjx.20250769
- VernacularTitle:基于XRD、FTIR、TG-DTA结合化学计量学鉴别白矾与铵明矾
- Author:
Bin WANG
1
;
Jingwei ZHOU
1
;
Huangsheng ZHANG
1
;
Jian FENG
2
;
Hanxi LI
1
;
Guorong MEI
2
;
Jiaquan JIANG
1
;
Hongping CHEN
1
;
Fu WANG
1
;
Yuan HU
1
;
Youping LIU
1
;
Shilin CHEN
1
;
Lin CHEN
1
Author Information
1. State Key Laboratory of Southwestern Chinese Medicine Resources，School of Pharmacy， Chengdu University of Traditional Chinese Medicine，Chengdu 611137，China
2. Sichuan Neo-green Pharmaceutical Technology Development Co. Ltd.，Pengzhou 611930，China
- Publication Type:Journal Article
- Keywords:
Alumen;
Ammonium alum;
X-ray diffraction（XRD）;
Fourier-transform infrared spectroscopy（FTIR）;
thermogravimetric-differential thermal analysis（TG-DTA）;
authenticity identification;
chemometrics
- From:
Chinese Journal of Experimental Traditional Medical Formulae
2025;31(13):178-186
- CountryChina
- Language:Chinese
-
Abstract:
ObjectiveTo establish the multi-technique characteristic profiles of Alumen by X-ray diffraction（XRD）， Fourier-transform infrared spectroscopy（FTIR） and thermogravimetric-differential thermal analysis（TG-DTA）， and to explore the spectral characteristics for rapid identification of Alumen and its potential adulterant， Ammonium alum. MethodsA total of 27 batches of Alumen samples from 8 production regions were collected for preliminary identification based on visual characteristics. The PDF standard cards of XRD were used to differentiate Alumen from A. alum， and the XRD characteristic profiles of Alumen were established， and then the common peaks were screened. Based on hierarchical clustering analysis（HCA） and orthogonal partial least squares-discriminant analysis（OPLS-DA）， the characteristic information that could be used for identification of Alumen was selected with variable importance in the projection（VIP） value>1. FTIR characteristic profiles of Alumen were established， and key wavenumbers for identification were screened by HCA and OPLS-DA with VIP value>1. Meanwhile， the thermogravimetric differences between Alumen and A. alum were analyzed by TG-DTA， and the thermogravimetric traits that could be used for identification were screened. ResultsAlumen and A. alum could not be effectively distinguished by traits alone. However， by comparing the PDF standard cards of XRD， 15 batches of Alumen and 12 batches of A. alum could be distinguished. In the XRD profiles， 10 characteristic peaks were confirmed， corresponding to diffraction angles of 14.560°， 24.316°， 12.620°， 32.122°， 17.898°， 34.642°， 27.496°， 46.048°， 40.697° and 21.973°. In the FTIR profiles， 4 wavenumber ranges（399.193-403.050， 1 186.010-1 471.420， 1 801.190-2 620.790， 3 612.020-3 997.710 cm-1） and 12 characteristic wavenumbers（1 428.994， 1 430.922， 1 432.851， 1 434.779， 1 436.708， 1 438.636， 1 440.565， 1 442.493， 1 444.422， 1 446.350， 1 448.279， 1 450.207 cm-1） were identified. In the TG-DTA profiles， there were characteristic decomposition peaks of ammonium ion and mass reduction features near 555.34 ℃ for A. alum. These characteristics could serve as important criteria for distinguishing the authenticity of Alumen. ConclusionXRD， FTIR and TG-DTA can be used to rapidly detect Alumen and A. alum， and combined with the discriminant features selected through chemometrics， the rapid and accurate identification of Alumen and A. alum can be achieved. The research findings provide new approaches for the rapid identification of Alumen.
