Method for improving precision and accuracy of trimethylsilyl ether derivatization-GC-MS determination of saccharide and carboxylic acid compounds in aerosol

Abstract

The invention discloses a method for improving precision and accuracy of trimethylsilyl ether derivatization-GC-MS determination of saccharide and carboxylic acid compounds in aerosol, belonging to the technical field of determination of saccharide and carboxylic acid compounds in the aerosol. By adopting the method, analysis determination is carried out by adopting a chromatographic column with a pre-column, and the sample is diluted at the minimal ratio before being sampled, so that the real content information in the sample is reserved, and the damage to the chromatographic column is reduced to the minimal extent. An experiment proves that accurate concentration information and good measurement accuracy can be obtained. In addition, blocked reaction in an ice bath at a low temperature after derivatization is creatively proposed, and diluting and even mixing operations are carried out at a low temperature in an uncapping manner, so that the loss of a siloxane derivative product in the sample is reduced, and the determination accuracy and the parallel precision are further ensured.

Description

technical field [0001] The invention belongs to the technical field of determination of aerosol components, and in particular relates to a method for determining sugars and carboxylic acid compounds in aerosol by trimethylsilyl ether derivatization-GC / MS and a method for improving the measurement precision and accuracy. Background technique [0002] Trimethylsilyl ether derivatization-GC / MS determination is a fast and effective method for the determination of polar compounds (mainly sugars and carboxylic acid compounds). It has very obvious advantages in the qualitative determination of compounds. However, there are still some problems in quantitative determination, mainly due to the influence of pyridine in the sample on the chromatographic column, which leads to poor derivatization effect or poor peak shape when measuring some samples, which affects the precision of quantification. degree and accuracy. [0003] The existing trimethylsilyl ether derivatization-GC / MS metho...

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Problems solved by technology

[0004] The above classic trimethylsilyl ether derivatization-GC / MS method for the determination of sugars and carboxylic acid compounds has the following problems in quantitative analysis: 1) Pyridine must be added as a catalyst in the derivatization, but pyridine in the derivatization product will obviously 2) The product after derivatization is a semi-volatile product, and there will be a part of the product during the measurement process of opening the bottle lost due to retention in the gas phase

As a result, the peak area of ​​the internal standard compound in the parallel samples varies greatly, which affects the measurement precision of the parallel samples

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