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

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
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
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

1. [1] Zheng G, Zhang Y, Nie T, et al. Sensor Actuat B-Chem, 2019, 291:362
2. [2] Luo B R, Wan X, Deng X L, et al. Chinese Journal of Chromatography, 2016, 34(5):473 罗碧容, 万旭, 邓兴亮, 等. 色谱, 2016, 34(5):473
3. [3] Li Y, Fang Y, Cao Z, et al. Appl Catal B-Environ, 2019, 250:150
4. [4] Wang X, Ding H, Yu X, et al. Talanta, 2019, 197:98
5. [5] Tsai W T. J Environ Sci, 2006, 24:225
6. [6] Wilson N K, Chuang J C, Morgan M K, et al. Environ Res, 2007, 103:9
7. [7] Zhang S H, Wu K B, Hu S S. Talanta, 2002, 58:747
8. [8] Lu D, Lin S X, Wang L T, et al. Electrochim Acta, 2012, 85:131
9. [9] Niu Z L, Zhang J, Wu D M, et al. Int J Environ Anal Chem, 2019, 99(5):444
10. [10] Wei L, Yan Y, Deng J, et al. J Brazil Chem Soc, 2018, 29(10):2137
11. [11] Dinesh M, Roopan S M, Selvaraj C I, et al. J Photoch Photobio B, 2018, 5:8973
12. [12] Kumar S P, Munusamy S, Muthamizh S, et al. Mater Today, 2016, 161:273
13. [13] Gao F F, Liu J Y, Lu W H, et al. Chinese Journal of Chromatography, 2018, 36(6):573 高芳芳, 刘军英, 鹿文慧, 等. 色谱, 2018, 36(6):573
14. [14] Song W W, Luo X L, Li G K, et al. Chinese Journal of Chromatography, 2017, 35(1):20 宋雯雯, 罗夏琳, 李攻科, 等. 色谱, 2017, 35(1):20
15. [15] Zheng Q, Lu Y, Ye Z, et al. J Zhejiang Univ-Sc B, 2018, 19 (9):726
16. [16] Zeng H, Lu W, Hao L, et al. New J Chem, 2018, 42 (24):20205
17. [17] Hu L, Peng F, Xia D, et al. ACS Sustain Chem Eng, 2018, 6 (12):17391
18. [18] Renuka M K, Gayathri V. J Photoch Photobio A:Chemistry, 2018, 353:477
19. [19] Huang Y, Jiao Y, Gao Y, et al. Anal Chim Acta, 2019, 1063:99
20. [20] Andreia C, Cornelia M, Oana C, et al. Farmacia, 2018, 66(5):831
21. [21] Zhang L, Wang S, Yang R, et al. Food Chem, 2019, 289:313
22. [22] Furugen A, Nishimura A, Kobayashi M, et al. J Pharmaceut Biomed, 2019, 168:83
23. [23] Hewelt-Belka W, Garwolińska D, Belka M, et al. Food Chem, 2019, 288:154
24. [24] Vicente A I, Caio J M, Sardinha J, et al. Tetrahedron, 2012, 68(2):670
25. [25] Zhao W J, Wang W J, Chang H, et al. J Chromatogr A, 2012, 1251:74
26. [26] Wang L, Yang C, Zhang Q, et al. J Sep Sci, 2013, 36(16):2664
27. [27] Zhang W, Zhang Y, Jiang Q, et al. Anal Chem, 2016, 88(21):10523
28. [28] Zhang W, Deng Z, Zhao W, et al. J Agric Food Chem, 2014, 62(26):6100

扫一扫看文章

计量

PDF下载量: 1
文章访问数: 117
HTML全文浏览量: 3

通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142

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

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

计量

文章相关

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处