拉曼光谱法快速测定矿物药石膏中二水硫酸钙的含量  

Rapid determination of calcium sulfate dihydrate in mineral gypsum by Raman spectroscopy

作　　者：彭艳[1] 张丽颖[1] 金阳[1] 杨钊 陆兔林[3] 金传山 都述虎[1] PENG Yan;ZHANG Li-ying;JIN Yang;YANG Zhao;LU Tu-lin;JIN Chuan-shan;DU Shu-hu(School of Pharmacy,Nanjing Medical University,Nanjing 211166,China;Joinative Traditional Chinese Medicine Industry Co.,Ltd.,Wuhan 430040,China;School of Pharmacy,Nanjing University of Chinese Medicine,Nanjing 210046,China;School of Pharmacy,Anhui University of Chinese Medicine,Hefei 230012,China)

机构地区：[1]南京医科大学药学院,南京211166 [2]九州天润中药产业有限公司,武汉430040 [3]南京中医药大学药学院,南京210046 [4]安徽中医药大学药学院,合肥230012

出　　处：《药物分析杂志》2021年第7期1266-1271,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：国家重点研发计划资助(2018YFC1707000)。

摘　　要：目的:建立一种用拉曼光谱技术快速测定石膏中二水硫酸钙含量的方法。方法:首先以硝酸钠作为内标,氯化钠作为填充剂,与石膏样品混合研磨均匀,在室温干燥条件下,压片,然后进行拉曼光谱测定。测定条件:激发波长780 nm,激光功率24 mW,光阑50μm slit,10倍物镜,曝光时间2 s,累积2次,扫描范围300-1700 cm^(-1)。结果:二水硫酸钙质量分数在5%-35%范围内与二水硫酸钙和硝酸钠的拉曼特征峰强度比值(I_(1007)/I_(1068))呈良好的线性关系,线性回归方程为Y=0.019X-0.0355,R^(2)=0.9994;低、中、高3个浓度的平均加样回收率分别为99.4%、97.9%、99.1%,RSD分别为1.5%、1.1%、1.3%;10个批次石膏的二水硫酸钙含量测定结果(97.8%-102.0%)与EDTA-2Na滴定法测定结果(98.8%-101.3%)经t检验无明显统计学差异(P=0.415,>0.05)。结论:本实验建立的拉曼光谱法操作简便快速,测得的石膏样品中二水硫酸钙含量准确,可以作为药用石膏质量控制的分析方法。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 50μm slit,the lens was 10×objective,the exposure time was 2 s,the accumulation was 2 times,and the scanning range was 300~1700 cm^(-1).Results:The peak intensity ratio(I_(1007)/I_(1068))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-0.0355,R^(2)=0.9994.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.

关 键 词：矿物药 石膏 二水硫酸钙 拉曼光谱 快速检测 含量测定 质量控制 

分 类 号：R917[医药卫生—药物分析学]