Objective: To establish a Raman spectroscopic method for rapid determining the content of calcium sulfate dihydrate in gypsum. Methods: Sodium nitrate as internal standard and sodium chloride as filler were first mixed with gypsum,which were grinded,compressed into tablets and analyzed by Raman spectrometer. Analytical conditions were as follows:the excitation wavelength was 780 nm,the laser power was 24 mW,the aperture was 50 μm slit,the lens was 10×objective,the exposure time was 2 s,the accumulation was 2 times,and the scanning range was 300~1 700 cm-1. Results: The peak intensity ratio( I1 007/I1 068) was used for the quantitative evaluation of the gypsum level and showed a good linear relationship with mass fraction of calcium sulfate dihydrate in the range of 5%-35%. The linear regression equation was Y=0.019X-0.035 5,R2=0.999 4. The average recoveries at low, medium and high concentrations were 99.4%,97.9% and 99.1%,with RSD of 1.5%,1.1% and 1.3%,respectively. There was no significant difference between the analytical results(97.8%-102.0%) and those(98.8%-101.3%) with EDTA-2Na titration method by t test( P=0.415,>0.05). Conclusion: The method is rapid and accurate. It can be used as a new analytical method for quality control of medicinal gypsum.
PENG Yan, ZHANG Li-ying, JIN Yang, YANG Zhao, LU Tu-lin, JIN Chuan-shan, DU Shu-hu
. Rapid determination of calcium sulfate dihydrate in mineral gypsum by Raman spectroscopy*[J]. Chinese Journal of Pharmaceutical Analysis, 2021
, 41(7)
: 1266
-1271
.
DOI: 10.16155/j.0254-1793.2021.07.18
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