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磺胺类同分异构体质谱裂解规律及色谱分离研究

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采用液相色谱-电喷雾-三重四极杆串联质谱法研究磺胺类同分异构体成分在电喷雾离子源正、负离子模式下的质谱裂解规律及分离方法.结果表明,一级质谱中,10种磺胺均在正离子模式下获得响应良好的[M+H]+.二级质谱中,磺胺类的裂解途径大多是发生在-SO2-两端,形成碎片离子[C6H6NSO2]+、[C6H6NO]+和[C6H6N]+,[C6H6N]+进一步裂解产生碎片离子[C5H5]+;类型2响应较高的碎片离子为m/z 124和m/z 186;类型3可形成碎片离子m/z 215和m/z 126.采用Thermo Scientific Hypersil GOLD C18色谱柱,柱温35℃,进样量20 µL,流动相为5 mmol/L乙酸铵(含0.1%甲酸)和甲醇,流速0.25 mL/min,在正离子扫描模式下,设置梯度洗脱程序分离了4个类型10种同分异构体.这些质谱裂解规律和分离方法有助于对磺胺类同分异构体的定性和定量分析提供理论依据.
Study on Mass Spectrometry Decomposition and Chromatographic Separation of Sulfonamide Isomers
Liquid chromatography electrospray ionization triple quadrupole tandem mass spectrometry was used to study the fragmentation rule and separation method of sulfonamide isomers in the positive and negative ion modes of electrospray ion source.The results showed that in the primary mass spectrometry,all 10 sulfonamides obtained well responsive[M+H]+ in the positive ion mode.In secondary mass spectrometry,the cleavage pathways of sulfonamides mostly occur at the ends of-SO2-,forming fragment ions[C6H6NSO2]+、[C6H6NO]+ and[C6H6N]+,[C6H6N]+ further cleavage of[C6H6N]+ produces fragment ions[C5H5]+;The fragment ions with higher response in type 2 are m/z 124 and m/z 186;Type 3 can form fragmented ions m/z 215 and m/z 126.Thermo Scientific Hypersil GOLD C18 chromatographic column was used,the column temperature was 35℃,the injection amount was 20µL,the mobile phase was 5mmol/L Ammonium acetate(containing 0.1%formic acid)and methanol,and the flow rate was 0.25mL/min.Under the positive ion scanning mode,gradient elution program was set to separate 4 types and 10 kinds of isomers.These mass spectrometry fragmentation patterns and separation methods contribute to providing theoretical basis for the qualitative and quantitative analysis of sulfonamide isomers.

sulfonamideisomerpyrolysis lawchromatographic separationliquid chromatography tandem mass spectrometry

黄鸾玉、吴祥庆、蒙源、江林源

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广西壮族自治区水产科学研究院,广西 南宁 530021

磺胺类 同分异构体 裂解规律 色谱分离 液相色谱-串联质谱法

广西科技重大专项广西农业科技自筹经费项目广西农业科技自筹经费项目

桂科AA20302019-1Z2023041Z2023042

2024

广州化学
中国科学院广州化学研究所

广州化学

影响因子:0.291
ISSN:1009-220X
年,卷(期):2024.49(2)
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