四氮杂杯[2]芳烃[2]三嗪键合硅胶固相萃取-高效液相色谱法测定河水中硝基苯酚和己烯雌酚

引用本文: 彭子芳, 李琴, 张光瑞, 赵无垛, 练鸿振, 张书胜. 四氮杂杯[2]芳烃[2]三嗪键合硅胶固相萃取-高效液相色谱法测定河水中硝基苯酚和己烯雌酚[J]. 色谱, 2020, 38(1): 143-148. doi: 10.3724/SP.J.1123.2019.06022 shu

Citation: PENG Zifang, LI Qin, ZHANG Guangrui, ZHAO Wuduo, LIAN Hongzhen, ZHANG Shusheng. Solid phase extraction and high performance liquid chromatography with tetraaza[2]arene[2]triazine-bonded silica gel adsorbent for determination of nitrophenols and diethylstilbestrol in river water[J]. Chinese Journal of Chromatography, 2020, 38(1): 143-148. doi: 10.3724/SP.J.1123.2019.06022 shu

四氮杂杯[2]芳烃[2]三嗪键合硅胶固相萃取-高效液相色谱法测定河水中硝基苯酚和己烯雌酚

彭子芳 ^1, ,
李琴 ^2,3, ,
张光瑞 ^1, ,
赵无垛 ^1, ,
练鸿振 ^3, ,
张书胜 ^{1,
,}

1.
郑州大学化学学院, 河南郑州 450001;
2.
郑州市食品药品检验所, 河南郑州 450008;
3.
南京大学化学化工学院, 江苏南京 210023

通讯作者: 张书胜,E-mail:zsszz@126.com

基金项目:
国家自然科学基金（21775140）.

摘要: 基于四氮杂杯[2]芳烃[2]三嗪键合硅胶吸附剂（NC-Si），构建了固相萃取-高效液相色谱法同时测定河水中3种硝基苯酚和己烯雌酚的新方法。考察并获得了固相萃取和液相色谱分离的优化条件：将样品溶液pH调至5，以5 mL/min上样，经自制固相萃取柱净化，2 mL氨水-甲醇（2：98，v/v）洗脱；在C8柱上以甲醇-0.1%磷酸溶液为流动相进行梯度洗脱。4种目标分析物的检出限（LOD，S/N=3）为0.03~0.3 μg/L，定量限（LOQ，S/N=10）为0.1~1.0 μg/L；加标回收率为75.5%~104.2%，相对标准偏差（RSD，n=5）小于6.3%。该方法准确、可靠，可用于河水中硝基苯酚及己烯雌酚的灵敏检测。

关键词:

English

Solid phase extraction and high performance liquid chromatography with tetraaza[2]arene[2]triazine-bonded silica gel adsorbent for determination of nitrophenols and diethylstilbestrol in river water

1.
College of Chemistry, Zhengzhou University, Zhengzhou 450001, China;
2.
Food and Drug Inspection Institute of Zhengzhou, Zhengzhou 450008, China;
3.
College of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210023, China

Corresponding author: ZHANG Shusheng, zsszz@126.com

Received Date: 25 June 2019
Fund Project:
National Natural Science Foundation of China (No. 21775140).

Abstract: A novel method based on solid phase extraction (SPE)-high performance liquid chromatography (HPLC) was developed for the simultaneous determination of nitrophenols and diethylstilbestrol in river water. Tetraaza[2]arene[2]triazine-bonded silica gel, a homemade SPE adsorbent, was used to enrich the nitrophenols and diethylstilbestrol, and the optimal SPE and HPLC conditions were established. The sample solution was adjusted to pH 5, purified with a lab-made solid phase extraction column, and then eluted with 2 mL ammonia-methanol (2:98, v/v). The enriched sample was separated on a C8 column with methanol and 0.1% phosphoric acid solution as mobile phases in a gradient elution. Under the optimized conditions, the limits of detection (LOD, S/N=3) for the four target analytes were 0.03-0.3 μg/L, and the limits of quantification (LOQ, S/N=10) were 0.1-1.0 μg/L. The recoveries were 75.5%-104.2%, and the relative standard deviations (RSD, n=5) were less than 6.3%. The proposed method is accurate and reliable, and it has been successfully used for determining nitrophenols and diethylstilbestrol in river water.

Key words:

tetraaza[2]arene[2]triazine
/ solid phase extraction(SPE)
/ high performance liquid chromatography (HPLC)
/ nitrophenol
/ diethylstilbestrol
/ river water

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四氮杂杯[2]芳烃[2]三嗪键合硅胶固相萃取-高效液相色谱法测定河水中硝基苯酚和己烯雌酚

通讯作者: 张书胜,E-mail:zsszz@126.com

English

Solid phase extraction and high performance liquid chromatography with tetraaza[2]arene[2]triazine-bonded silica gel adsorbent for determination of nitrophenols and diethylstilbestrol in river water

Corresponding author: ZHANG Shusheng, zsszz@126.com

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

四氮杂杯[2]芳烃[2]三嗪键合硅胶固相萃取-高效液相色谱法测定河水中硝基苯酚和己烯雌酚

通讯作者: 张书胜,E-mail:zsszz@126.com

English

Solid phase extraction and high performance liquid chromatography with tetraaza[2]arene[2]triazine-bonded silica gel adsorbent for determination of nitrophenols and diethylstilbestrol in river water

Corresponding author: ZHANG Shusheng, zsszz@126.com

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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