管内硼亲和固相微萃取-高效液相色谱全自动在线联用检测茶饮料中的顺式二羟基化合物

doi:10.3724/SP.J.1123.2019.06020

色谱 ›› 2020, Vol. 38 ›› Issue (1): 137-142.DOI: 10.3724/SP.J.1123.2019.06020

管内硼亲和固相微萃取-高效液相色谱全自动在线联用检测茶饮料中的顺式二羟基化合物

王欣, 何坚刚, 罗琪, 刘震()

南京大学化学化工学院, 生命分析化学国家重点实验室, 江苏南京 210023

收稿日期:2019-06-24 出版日期:2020-01-08 发布日期:2020-12-11
通讯作者: 刘震
作者简介:刘震, Tel:(025)89685639, E-mail:zhenliu@nju.edu.cn
基金资助:
国家自然科学基金面上项目(21075063)

Automated hyphenation of in-tube boronate affinity solid-phase microextraction with high performance liquid chromatography for the determination of cis-diol compounds in tea beverages

WANG Xin, HE Jiangang, LUO Qi, LIU Zhen()

State Key Lab of Analytical Chemistry for Life Science, School of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210023, China

Received:2019-06-24 Online:2020-01-08 Published:2020-12-11
Contact: LIU Zhen
Supported by:
General Grant from the National Natural Science Foundation of China(21075063)

摘要/Abstract

摘要：

自动化联用分析技术对于降低人力强度、提高效率和保证数据重现性等具有重要意义。硼亲和固相微萃取（BA-SPME）是近十年出现的用于富集顺式二羟基化合物的独特工具，但BA-SPME与高效液相色谱（HPLC）的自动化在线联用还未见报道。该文报道了一种新颖的管内BA-SPME-HPLC全自动在线联用方法，用于分析茶饮料中的顺式二羟基化合物。该自动化在线联用方法利用自动进样器通过六通阀的切换实现流路连接。制备了管内BA-SPME毛细管，考察了涂层柱的柱容量，并对其形貌进行了表征，考察并优化了影响实际样品分离效果的因素。最后，利用该联用方法对3种不同品牌的茶饮料进行了分析，并对沏茶温度对茶水中顺式二羟基化合物含量的影响进行了评价。

关键词: 硼亲和, 液相色谱, 自动化在线联用, 固相微萃取, 顺式二羟基化合物, 茶饮料

Abstract:

Automatic hyphenated analytical techniques hold great promise for reducing labour intensity, enhancing efficiency, and ensuring data reproducibility. In recent decade, Boronate affinity solid phase microextraction (BA-SPME) has emerged as a unique tool for the selective extraction of cis-diol-containing compounds. However, automatic hyphenation of SPME with high performance liquid chromatography (HPLC) has not yet been reported. Herein we report a new automated hyphenation of in-tube BA-SPME with HPLC for the determination of cis-diol compounds in tea beverages. The automated hyphenation was implemented through a flow-switch via the six-way valve of an autosampler. We prepared an in-tube SPME capillary, investigated the loading capacity of the coated column, characterized the morphology of the column, and investigated the factors influencing the separation. Finally, using the automatic hyphenated SPME-HPLC approach, we analyzed the cis-diol-containing compounds in three kinds of commercial tea beverages and investigated the effect of tea-making temperature on the content of the cis-diol-containing compounds in the prepared tea.

Key words: boronate affinity, liquid chromatography (LC), automated on-line hyphenation, solid phase microextraction (SPME), cis-diol compounds, tea beverage

王欣, 何坚刚, 罗琪, 刘震. 管内硼亲和固相微萃取-高效液相色谱全自动在线联用检测茶饮料中的顺式二羟基化合物[J]. 色谱, 2020, 38(1): 137-142.

WANG Xin, HE Jiangang, LUO Qi, LIU Zhen. Automated hyphenation of in-tube boronate affinity solid-phase microextraction with high performance liquid chromatography for the determination of cis-diol compounds in tea beverages[J]. Chinese Journal of Chromatography, 2020, 38(1): 137-142.

图/表 7

图1 管内硼亲和固相微萃取-液相色谱自动在线联用原理示意图

Fig. 1 Schematic diagram of automated on-line hyphenation of in-tube solid phase microextraction (SPME) with HPLC a. Extraction (Step 1): from the sample vial, the sample solution is repeatedly drawn into and ejected out of the in-tube SPME capillary; b. desorption and separation (Step 2): the in-tube SPME capillary is connected with the HPLC system.

图2 聚合反应的原理图

Fig. 2 Schematic of the copolymerization reaction AIBN: 2, 2′-azobis(2-methylpropionitrile).

图3 固相微萃取毛细管的扫描电镜图

Fig. 3 Scanning electron microscope (SEM) images of the SPME capillary a. cross-sectional view of the capillary; b. enlarged image of the edge of the inner surface of the capillary.

图4 流速对茶饮料样品中顺式二羟基化合物的分离的影响

Fig. 4 Effects of the flow rate of the mobile phase on the separation of cis-diol compounds extracted from tea beverage samples

图5 有无固相微萃取时的HPLC色谱图对比

Fig. 5 Comparison of the HPLC chromatograms with and without SPME

图6 不同茶饮料样品的色谱对比图

Fig. 6 Comparison of the chromatograms for different tea beverages

图7 沏茶温度对茶水中顺式二羟基化合物的影响

Fig. 7 Effects of tea-making temperature on the profile of cis-diol compounds in tea

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管内硼亲和固相微萃取-高效液相色谱全自动在线联用检测茶饮料中的顺式二羟基化合物

Automated hyphenation of in-tube boronate affinity solid-phase microextraction with high performance liquid chromatography for the determination of cis-diol compounds in tea beverages

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