镍钛合金纤维/有机硅-聚氨酯固相微萃取头的制备及其在水中7种取代苯化合物检测中的应用

引用本文: 申书昌, 任芳秀, 吕伟超. 镍钛合金纤维/有机硅-聚氨酯固相微萃取头的制备及其在水中7种取代苯化合物检测中的应用[J]. 色谱, 2018, 36(12): 1323-1329. doi: 10.3724/SP.J.1123.2018.08047 shu

Citation: SHEN Shuchang, REN Fangxiu, LÜ Weichao. Preparation of nickel-titanium alloy fiber/organosilicone-polyurethane solid phase microextraction head and its application to the determination of seven substituted benzenes in water[J]. Chinese Journal of Chromatography, 2018, 36(12): 1323-1329. doi: 10.3724/SP.J.1123.2018.08047 shu

镍钛合金纤维/有机硅-聚氨酯固相微萃取头的制备及其在水中7种取代苯化合物检测中的应用

齐齐哈尔大学分析测试中心, 黑龙江齐齐哈尔 161006
基金项目:
黑龙江省教育厅基本科研业务专项（135209221）.

摘要: 以2，4-甲苯二异氰酸酯、聚酯多元醇、羟基硅油为原料，辛酸亚锡为催化剂，环己酮为溶剂，合成有机硅-聚酯型聚氨酯。将此聚合物涂于经氢氧化钾水热处理的镍钛合金纤维丝表面作为固相微萃取涂层，制得固相微萃取头。利用红外光谱法分析了聚合物结构；热重分析法确定了涂层最高使用温度；扫描电子显微镜观察了萃取头的表面形貌。以顶空萃取-固相微萃取-气相色谱法（HS-SPME-GC）测定了水中甲苯、二甲苯、间二氯苯、邻二氯苯、苯甲酸乙酯、硝基苯、苯甲醇7种取代苯化合物的含量。各被测物的色谱峰面积与其质量浓度呈良好的线性关系，相关系数（R²）为0.9926~0.9998，方法的检出限为0.08~0.24 μg/L。实际样品测定的加标回收率为95.9%~105.4%，相对标准偏差为1.4%~5.0%。通过对实际样品的分析，说明制备的固相微萃取头涂层不易脱落、性质稳定，对于水中取代苯类化合物具有很强的吸附能力。

关键词:

English

Preparation of nickel-titanium alloy fiber/organosilicone-polyurethane solid phase microextraction head and its application to the determination of seven substituted benzenes in water

Analytical and Testing Center of Qiqihar University, Qiqihar 161006, China
Received Date: 29 August 2018
Fund Project:
Special Research Project of Heilongjiang Province Education Office (No. 135209221).

Abstract: Toluene-2,4-diisocyanate, polyester polyol, and hydroxy silicone oil were used as raw materials; stannous octoate was used as the catalyst; and cyclohexanone was used as the solvent to synthesize organosilicone-polyurethane (SP). The polymer was coated on the surface of a nickel-titanium alloy fiber treated hydrothermally with potassium hydroxide. It was the prepared for headspace solid phase microextraction (HS-SPME). The polymer structure was analyzed by infrared spectroscopy, the highest temperature of the coating was determined by thermogravimetric analysis, and the surface morphology of the extraction head was observed by scanning electron microscopy. The benzene series of toluene, xylene, m-dichlorobenzene, o-dichlorobenzene, ethyl benzoate, nitrobenzene and benzyl alcohol in water were determined by HS-SPME-gas chromatography (GC) method. There was a good linear relationship between the chromatographic peak area and mass concentration of each measured object. The correlation coefficients (R²) were 0.9926-0.9998. The limits of detection were 0.08-0.24 μg/L. The recoveries of the spiked samples were 95.9%-105.4%, and the relative standard deviations were 1.4%-5.0%. The coating of SPME head adhered more firmly, and had a better adsorption performance for the substituted benzenes in water.

Key words:

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镍钛合金纤维/有机硅-聚氨酯固相微萃取头的制备及其在水中7种取代苯化合物检测中的应用

English

Preparation of nickel-titanium alloy fiber/organosilicone-polyurethane solid phase microextraction head and its application to the determination of seven substituted benzenes in water

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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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

镍钛合金纤维/有机硅-聚氨酯固相微萃取头的制备及其在水中7种取代苯化合物检测中的应用

English

Preparation of nickel-titanium alloy fiber/organosilicone-polyurethane solid phase microextraction head and its application to the determination of seven substituted benzenes in water

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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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs