Purification method of HPLC-grade tert-butyl methyl ether for LC-MS

Abstract

The invention discloses a purification method of HPLC-grade tert-butyl methyl ether for LC-MS, and relates to the technical field of biology and new medicine. The purification method comprises: adding 30 L of a common HPLC grade methanol raw material and 100 G of a silica gel bonded phase metal removing agent with a product code of SI-THU to a 50 L customized glass reaction container, wherein the bottom of the container is provided with a valve for coupling with a filtration device; inserting a glass connection tube to the bottom of the container, opening a N2 cylinder valve, introducing N2, and stirring; and carrying out a reaction for 4-8 h, sampling, carrying out equipment detection, stopping stirring when the regulated index is achieved, and carrying out filtration package. With the purification method, characteristics of high product purity, low cost, good batch stability and stable quality are provided, and analysis requirements of high performance liquid chromatography LC-MS with high requirements can be met.

Description

Technical field: [0001] The invention relates to the technical field of biology and new medicine, in particular to a method for purifying HPLC grade tert-butyl methyl ether for LC-MS. Background technique: [0002] The HPLC mobile phase that controls metals and heavy metal ions is particularly important in liquid chromatography analysis, especially in LC-MS applications, because it directly affects the accuracy of test results and the service life of instrument chromatographic columns; so domestic chromatography The use of HPLC-grade tert-butyl methyl ether in the detection field puts forward new requirements; in my country, the control of metal and heavy metal ions in HPLC reagents is not controlled due to the limitation of domestic purification technology; most experimenters use HPLC-grade LC imported from Europe and America. -MS tert-butyl methyl ether; however, due to the high cost of use, the experimenters have to use ordinary HPLC tert-butyl methyl ether for transition; ...

AI Technical Summary

Problems solved by technology

[0002] The HPLC mobile phase that controls metal and heavy metal ions is particularly important in liquid chromatography analysis, especially in LC-MS applications, because it directly affects the accuracy of test results and the service life of instrument chromatographic columns; so domestic chromatography The use of HPLC-grade tert-butyl methyl ether in the detection field puts forward new requirements; in my country, the control of metal and heavy metal ions in HPLC reagents is not controlled due to the limitation of domestic purification technology; most experimenters use HPLC-grade LC imported from Europe and America. -MS tert-butyl methyl ether; however, due to the high cost of use, the experimenters have to use ordinary HPLC tert-butyl methyl ether for transition; however, the technical indicators of domestic solvents are generally lower than those in Europe and the United States, the quality is unstable, and the batch reproducibility is not good

The unfavorable factor is that ordinary HPLC-grade methanol does not control metal and heavy metal ions. After a large amount of mobile phase flows into the HPLC system, the expensive HPLC-specific LC-MS chromatographic column used by LC-MS is damaged by metal ions. Ineffective due to poisoning, and some even affect the separation effect