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

作　　者：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[3] 陈亮[1] WANG Xinyu;LONG Qilai;WANG Luning;MA Liujin;XU Jiani;LIU Ting;WANG Yifei;HUANG Feifei;GUO Jianming;CHEN Bo;CHEN Liang(College of Biological and Environmental Sciences,Ningbo,Zhejiang 315100,China;Department of Urology,Zhongshan Hospital,Fudan University,Shanghai 200032,China;Key Laboratory of the Ministry of Public Health and Safety Education,School of Public Health,Fudan University,Shanghai 200032,China)

机构地区：[1]浙江万里学院生物与环境学院,浙江宁波315100 [2]复旦大学附属中山医院泌尿外科,上海200032 [3]复旦大学公共卫生学院,公共卫生安全教育部重点实验室,上海200032

出　　处：《上海预防医学》2022年第8期820-824,共5页Shanghai Journal of Preventive Medicine

基　　金：国家级2020大学生创新创业项目(202010876028);浙江省公益技术研究计划/分析测试项目(LGC20B050005)。

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。[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 at 1∶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 MELUA 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.

关 键 词：草酸钙结石 三聚氰胺 三聚氰酸 尿酸 傅里叶变换红外光谱 二次二阶导数 

分 类 号：R115[医药卫生—公共卫生与预防医学]