傅里叶导数红外光谱法测定草酸钙结石中三聚氰胺及其结合物

王欣雨; 龙启来; 王泸宁; 麻柳缙; 徐佳妮; 刘婷; 王艺菲; 黄菲菲; 郭剑明; 陈波; 陈亮

doi:10.19428/j.cnki.sjpm.2022.21529

傅里叶导数红外光谱法测定草酸钙结石中三聚氰胺及其结合物

Determination of melamine and its conjugates in calcium oxalate stones by Fourier transform infrared spectroscopy

摘要

摘要:
目的利用二阶导数傅里叶红外光谱（FTIR）建立分析人体泌尿结石中三聚氰胺（MEL）、三聚氰胺与三聚氰酸结合物（MEL-CYA）、三聚氰胺与尿酸结合物（MEL⁃UA）的方法。
方法通过向草酸钙（CaO_x）结石标本中加入MEL、MEL⁃CYA、MEL⁃UA制成样品，用FTIR的一维谱图和二次二阶导数谱图分析其中MEL及其结合物的特征基团信息，筛选出可用于判断结石中可能存在MEL及其结合物的特征响应波段，并确定其检出比例。
结果当CaO_x结石中掺杂MEL单体时，导数谱图以1 548 cm^-1为其特征峰，最低检出比例可达MEL与CaO_x结石的质量比1∶100（即1.0%）；当CaO_x结石中掺杂MEL⁃CYA时，导数谱图以1 740 、1 538 cm^-1为其特征峰，最低检出比例可达MEL⁃CYA与CaO_x结石的质量比1∶500（即0.2%）；当CaO_x结石中掺杂MEL⁃UA时，导数谱图以1 117、982、710 cm^-1为其特征峰，最低检出比例可达MEL⁃UA与CaO_x结石的质量比1∶250（即0.4%）。
结论 FTIR的二次二阶导数谱图相较于一维谱图，其检测CaO_x结石中MEL含量的最低检出比例可达0.2%~1.0%，其检测MEL的特征响应峰和最低检出比例基本满足结石中微量MEL的检测要求，可为MEL在结石中的红外光谱分析提供有益的借鉴。

Abstract:
Objective To establish a method of two-times second derivative Fourier transform infrared spectroscopy （FTIR） for identifying melamine （MEL） and its conjugates with cyanuric acid （MEL-CYA） or with uric acid （MEL-UA） in human urinary calculi.
Methods MEL， MEL-CYA and MEL-UA were added to calcium oxalate stone samples， and then analyzed by two-times second derivative FTIR for identifying the characteristic response bands of MEL and its conjugates in stones as well as confirming the ratio of detection.
Results The second derivative FTIR could improve the detection of MEL in CaO_x stones by two orders of magnitude. When CaO_x being mixed with MEL （MEL∶ CaO_x）， the two-times second derivative FTIR showed the characteristic peak at 1 548 cm^-1 and the minimum mass ratio of detection at1∶100 （1%）. When CaO_x being mixed with MEL-CYA complex （MEL-CYA∶ CaO_x）， the two-times second derivative FTIR showed the characteristic peak on 1 740 cm^-1 and 1 538 cm^-1 and the minimum mass ratio of detection at 1∶500 （0.2%）. When CaO_x being mixed with MEL-UA complex （MEL-UA∶ CaO_x）， the two-times second derivative FTIR showed the characteristic peak at 1 117， 982 and 710 cm^-1 and the minimum mass ratio of detection at 1∶250 （0.4%）.
Conclusion Compare to the original spectra， the two-times second derivative FTIR can improve the detection ratio MEL in the CaO_x stones from 0.2% to 1.0%. The second derivative FTIR has the unique characteristic bands and sensitive detection limit for identifying MEL in kidney stones.

HTML全文

参考文献(15)

施引文献

资源附件(0)