内部萃取电喷雾电离质谱直接分析脐橙

doi:10.7503/cjcu20150233

高等学校化学学报 ›› 2015, Vol. 36 ›› Issue (10): 1912.doi: 10.7503/cjcu20150233

内部萃取电喷雾电离质谱直接分析脐橙

卢海艳, 张华, 周鹏, 杨美玲, 钟涛, 姚国灿, 陈焕文()

东华理工大学, 江西省质谱科学与仪器重点实验室, 南昌 330013

收稿日期:2015-03-25 出版日期:2015-10-10 发布日期:2015-09-14
作者简介:联系人简介: 陈焕文, 男, 博士, 教授, 博士生导师, 主要从事质谱分析研究. E-mail:chw8868@gmail.com
基金资助:
长江学者和创新团队发展计划项目(批准号: IRT13054)和国家自然科学基金(批准号: 31370384, 21225522)资助

Direct Analysis of Navel Orange Using Internal Extractive Electrospray Ionization Mass Spectrometry^†

LU Haiyan, ZHANG Hua, ZHOU Peng, YANG Meiling, ZHONG Tao, YAO Guocan, CHEN Huanwen^*()

Jiangxi Key Laboratory for Mass Spectrometry and Instrumentation,East China Institute of Technology, Nanchang 330013, China

Received:2015-03-25 Online:2015-10-10 Published:2015-09-14
Contact: CHEN Huanwen E-mail:chw8868@gmail.com
Supported by:
† Supported by the Program for Changjiang Scholars and Innovative Research Team in University, China(No;IRT13054) and the National Natural Science Foundation of China(Nos.31370384, 21225522)

摘要/Abstract

摘要：

在正离子模式下, 分别对不同品质脐橙的内果皮和果肉进行了内部萃取电喷雾电离质谱(iEESI-MS)分析, 在未经过预处理的前提下直接获得了72个脐橙内果皮样品和72个脐橙果肉样品在m/z 50~2000范围内的化学指纹谱图, 鉴定了脐橙组织中氨基酸、糖类和生物碱等重要化学成分. iEESI-MS化学指纹谱图表明, 脐橙的果肉与内果皮组织中脯氨酸和糖类等成分的组成具有一定的相似性, 而其它化学组分(如水苏碱、辛弗林等)在2类组织中的含量差异明显. 主成分分析(PCA)结果表明, 样品的iEESI-MS指纹谱图与该脐橙的品质相关, 与样品的实际品质差异一致. 因此, iEESI-MS可直接获得不同品质脐橙差异性化学成分的信息, 从分子水平上判断脐橙品质的优劣.

关键词: 内部萃取电喷雾电离质谱, 脐橙, 品质, 直接分析

Abstract:

Internal extractive electrospary ionization mass spectrometry(iEESI-MS) was applied on the assessment of navel orange quality without any sample pretreatment. Both endocarp tissues(72 samples) and flesh tissues(72 samples) of navel oranges from three habitats were interrogated directly by iEESI-MS at mass range of m/z 50—2000. A fused silicon capillary was inserted into the navel orange tissue, allowing a distance of 2 mm between the fused silicon capillary tip and the sample apex. The apex of the sample was pointed to the mass spectrometer ion inlet intentionally with a distance of 4—5 mm. Extraction solvent biased with a high voltage(4.5 kV) was injected through the fused silicon capillary into the navel orange tissue at a flow rate of 2 μL/min, producing charged fine droplets containing chemicals toward the adjacent mass spectrometer inlet. Chemical constituents such as sugars, amino acids, vitamin and alkaloids were simultaneously extracted from the navel orange tissue, and identified through collision-induced dissociation(CID) experiment. Furthermore, mass spectral fingerprints were processed by principal component analysis(PCA) to visualize the quality differences. Our experimental results indicated that iEESI-MS can directly characterize the quality differences of navel oranges by molecular analysis. The merits of iEESI-MS include simplicity, good specificity, high throughput and minimum sample pretreatment.

Key words: Internal extractive electrospary ionization mass spectrometry, Navel orange, Quality assessment, Direct analysis

TrendMD:

卢海艳, 张华, 周鹏, 杨美玲, 钟涛, 姚国灿, 陈焕文. 内部萃取电喷雾电离质谱直接分析脐橙. 高等学校化学学报, 2015, 36(10): 1912.

LU Haiyan, ZHANG Hua, ZHOU Peng, YANG Meiling, ZHONG Tao, YAO Guocan, CHEN Huanwen. Direct Analysis of Navel Orange Using Internal Extractive Electrospray Ionization Mass Spectrometry^†. Chem. J. Chinese Universities, 2015, 36(10): 1912.

图/表 7

Fig.1 Schematic diagram of iEESI-MS

Fig.2 iEESI-MS spectra of orange flesh from different habitats(A) Guoxi; (B) Anxi; (C) Yongxing.

Fig.3 MS2 spectra of choline(A), proline(B), stachydrine(C) and sucrose(D) from orange flesh

Fig.4 PCA score plots(A) and PCA loading plots(B) of iEESI-MS data of orange flesh from different habitats a. Guoxi; b. Anxi; c. Yongxing.

Fig.5 iEESI-MS spectra of orange endocarp from different habitats(A) Guoxi; (B) Anxi; (C) Yongxing.

Table 1 Summary of the dominant chemicals in navel orange from different habitats detected by iEESI-MS*

Habitat	Sampling position	Dominant mass spectra peaks
		m/z 104	m/z 116	m/z 144	m/z 168	m/z 175	m/z 219	m/z 381	m/z 403
		Choline	Proline	Stachydrine	Synephrine	Arginine	Glucose/ fructose	Sucrose	Nobiletin
		C₅H₁₄NO⁺	C₅H₁₀N $O 2 +$	C₇H₁₀N $O 2 +$	C₉H₁₄N $O 2 +$	C₆H₁₅N₄ $O 2 +$	C₆H₁₂O₆K⁺	C₁₂H₂₂O₆K⁺	C₂₁H₂₃ $O 8 +$
Guoxi	Flesh	+	++	++++	+	+	++++	+++	+
	Endocarp	+	++	+++	++++	+	++++	++	+
Anxi	Flesh	+	++	++++	+	+	+++	+++	+
	Endocarp	+	++	+++	++++	+	++++	+++	+
Yongxing	Flesh	+	+++	+++	+	+	++++	+++	+
	Endocarp	+	+	++	+++	+	++++	+	+

Table 1 Summary of the dominant chemicals in navel orange from different habitats detected by iEESI-MS*

Habitat	Sampling position	Dominant mass spectra peaks
		m/z 104	m/z 116	m/z 144	m/z 168	m/z 175	m/z 219	m/z 381	m/z 403
		Choline	Proline	Stachydrine	Synephrine	Arginine	Glucose/ fructose	Sucrose	Nobiletin
		C₅H₁₄NO⁺	C₅H₁₀N $O 2 +$	C₇H₁₀N $O 2 +$	C₉H₁₄N $O 2 +$	C₆H₁₅N₄ $O 2 +$	C₆H₁₂O₆K⁺	C₁₂H₂₂O₆K⁺	C₂₁H₂₃ $O 8 +$
Guoxi	Flesh	+	++	++++	+	+	++++	+++	+
	Endocarp	+	++	+++	++++	+	++++	++	+
Anxi	Flesh	+	++	++++	+	+	+++	+++	+
	Endocarp	+	++	+++	++++	+	++++	+++	+
Yongxing	Flesh	+	+++	+++	+	+	++++	+++	+
	Endocarp	+	+	++	+++	+	++++	+	+

Fig.6 PCA score plots(A) and PCA loading plots(B) of iEESI-MS data of orange endocarp from different habitats

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内部萃取电喷雾电离质谱直接分析脐橙

Direct Analysis of Navel Orange Using Internal Extractive Electrospray Ionization Mass Spectrometry^†

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内部萃取电喷雾电离质谱直接分析脐橙

Direct Analysis of Navel Orange Using Internal Extractive Electrospray Ionization Mass Spectrometry†

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Direct Analysis of Navel Orange Using Internal Extractive Electrospray Ionization Mass Spectrometry^†