调控微波等离子体能量进行药片活性分子结构的质谱分析

doi:10.7503/cjcu20160686

摘要/Abstract

摘要：

采用微波等离子体质谱(MPT-MS)技术, 对替硝唑和马来酸氯苯那敏药片进行快速质谱分析. 通过调控等离子体能量, 在一级谱图中可得到目标物的准分子离子及丰富的碎片离子, 这些碎片离子与其对应串联质谱数据基本一致, 甚至更加丰富; 结合标准品比对分析, 最终确定这些碎片离子来自目标物而非基质. 因此, MPT兼具硬电离和软电离性质, 采用MPT-MS技术从一级质谱图中获得的数据可对药片中活性分子的结构进行鉴定. 该方法具有快速、准确及环保等特点, 在发展MPT与简单的质量分析器联用, 实现质谱仪的小型化等方面有广阔的应用前景.

关键词: 微波等离子体炬, 质谱, 微波功率, 药片

Abstract:

A microwave plasma torch mass spectrometry(MPT-MS) method was applied for the qualitative analysis of active ingredients in tinidazole and chlorpheniramine tablets. By changing the microwave power, both the parent ion and abundant fragment ions of the target were obtained in the full-scan mass spectra. These fragment ions were in accordance with the fragments from tandem mass spectrometry experiments, and even more abundant. Therefore, MPT source, with both hard ionization and soft ionization properties, could be used for the fast qualitative analysis of active ingredients in tablets, because it can obtain both parent and fragment ions in the full-scan mass spectrometry experiments. This rapid, accuracy, and no pollution MPT-MS method is useful for developing MPT coupled to a simple mass analyzer and realizing the miniaturization of mass spectrometer.

Key words: Microwave plasma torch, Mass spectrometry, Microwave power, Tablet

中图分类号:

O657.6

TrendMD:

王新晨, 杨美玲, 张小平. 调控微波等离子体能量进行药片活性分子结构的质谱分析. 高等学校化学学报, 2017, 38(4): 561.

WANG Xinchen, YANG Meiling, ZHANG Xiaoping. Rapid Qualitative Analysis of Active Molecules in Tablets Using Microwave Plasma Torch Mass Spectrometry by the Regulation of Power^†. Chem. J. Chinese Universities, 2017, 38(4): 561.

图/表 8

Fig.1 Schematic of the MPT-MS setup

Fig.2 Full-scan mass spectra obtained by MPT-MS for tinidazole tablet(A, B) and tinidazole standard(C, D) at microwave powers of 30 W(A, C) and 130 W(B, D)

Fig.3 MS2 spectrum of tinidazole at m/z 248(A) and MS2 spectrum of chlorpheniramine at m/z 275(B)Insets of (A) are the MS3 spectra of m/z 248→m/z 202 and m/z 248→m/z 121); inset of (B) is the MS3 spectrum of m/z 275→230.

Fig.4 Proposed fragment pathways of [M+H]+ at m/z 248 for tinidazole

Table 1 Fragment ions of tinidazole and chlorpheniramine obtained by tandem MS

Tablet	Molecular weight	[M+H]⁺, m/z	MS², m/z	MS³, m/z
Tinidazole	247	248^a	202^b, 110	110
			128, 121^b	93
Chlorpheniramine	274	275^a	230^b	202, 167

Fig.5 Full-scan mass spectra obtained by MPT-MS for chlorpheniramine tablet(A, B) and chlorpheniramine standard(C, D) at microwave powers of 30 W(A, C) and 110 W(B, D)

Fig.6 Proposed fragmentation mechanism pathways of [M+H]+ at m/z 275 for chlorpheniramine

Fig.7 Effects of microwave power on the intensities of ions from active ingredients in tables by MPT-MS (A) Tinidazole; (B) chlorpheniramine.

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