差示扫描量热法测定4-正辛基酚、炔雌醇等5种化合物的纯度  

Purity Determination of Five Typical Endocrine Disrupting Compounds by Differential Scanning Calorimetry

作　　者：张思遥 李晓敏[1] 王海峰[1] 陈东梁 张庆合[1] ZHANG Siyao;LI Xiaomin;WANG Haifeng;CHEN Dongliang;ZHANG Qinghe(National Institute of Metrology,Beijing 100029,China;Beijing University of Chemical Technology,Beijing 100029,China)

机构地区：[1]中国计量科学研究院,北京100029 [2]北京化工大学,北京100029

出　　处：《计量科学与技术》2022年第7期22-27,共6页Metrology Science and Technology

基　　金：国家重点研发计划(2019YFC1604803)。

摘　　要：4-正辛基酚、4-正壬基酚、炔雌醇、己烷雌酚和双烯雌酚属于内分泌干扰物,在水体、土壤、食品中均有检出,其纯度标准物质具有广泛的市场需求。本文通过差示扫描量热法(DSC)对4-正辛基酚等5种有机化合物的纯度进行测定,并采用高效液相色谱法(HPLC)和热重分析法(TGA)对差示扫描量热法测量结果进行验证。结果表明,4-正辛基酚、4-正壬基酚、炔雌醇、己烷雌酚这4种雌激素的纯度可采用差示扫描量热法进行测定,且与高效液相色谱法的结果一致性较好。双烯雌酚由于没有明显的DSC吸热曲线,结合热重分析法发现双烯雌酚在熔融时分解,因此不能用DSC对其进行纯度测定。As endocrine-disrupting compounds, 4-octylphenol, 4-nonylphenol, ethinylestradiol, hexestrol, and dienestrol have been detected in water, soil and food, and their certified reference materials are in wide market demand. In this paper,the purity of the five organic compounds was analyzed by differential scanning calorimetry(DSC), and joint research was carried out by high-performance liquid chromatography(HPLC) and thermal gravimetric analysis(TGA). The results showed that the purity of 4-octylphenol, 4-nonylphenol, ethinylestradiol, and hexestrol could be determined by DSC, and the results were in good agreement with those of the HPLC method. Since there was no obvious endothermic curve of dienestrol observed by DSC combined with TGA which revealed the decomposition of dienestrol during melting. It is concluded that the DSC method is not applicable for the purity analysis of dienestrol.

关 键 词：差示扫描量热法 热重分析法 内分泌干扰物 纯度分析 

分 类 号：O657.72[理学—分析化学] TQ075[理学—化学]