Wang, Hui;Shao, Hong-xia;Qin, Qiu-ming published 《Determination of 2,5-dimethyl-2,5-hexanediol in process components of voriconazole products for injection by UPLC-MS/MS》. The research results were published in《Zhejiang Huagong》 in 2021.Application In Synthesis of 2,5-Dimethyl-2,5-hexanediol The article conveys some information:
Objective: To establish an ultra high performance liquid phase-tandem mass spectrometry (UPLC-MS/MS) method for the determination of 2,5-dimethyl-2,5-hexanediol (DHD) in process components of voriconazole for injection. Methods: The sample was redissolved by water and added with internal standard 2-methylpentane-2,4-diol (MPD), extracted with acetonitrile and injected. The liquid mass spectrometer was used for anal. The mobile phase A was methanol, and mobile phase B was 0.1% ammonia solution Column ACQUITY UPLC BEH Ph (2.1 mm×50 mm, 1.7 μm) was used for separation Electrospray ionization source and multiple reaction monitoring (MRM) mode were used for neg. ion scanning detection. Results: DHD showed a good linearity within between 10.0-68.0 μg·L-1 (r = 0.9990). The relative average deviation (RSD) of repeatability test was 1%, and the method recovery rate was 84-107%. The lower limit of detection (S/N ≈ 3) was 3.3 ppb, and the lower limit of quantification (S/N ≈ 10) was 10.0 ppb. The sample solution was stable in 24 h at room temperature Conclusion: UPLC-MS/MS method has many advantages, such as high sensitivity, accurate determination results, strong specificity and so on. UPLC-MS/MS method can be applied to the risk monitoring of DHD in process components of voriconazole for injection, and can provide a reference for the detection of DHD in other products. The experimental procedure involved many compounds, such as 2,5-Dimethyl-2,5-hexanediol (cas: 110-03-2) .
2,5-Dimethyl-2,5-hexanediol(cas:110-03-2) on heteropoly acid catalyzed dehydration yields cyclic ethers via stereospecific intramolecular SN2 mechanism. It reacts with nitriles in concentrated sulfuric acid to yield Δ1-pyrrolines.Application In Synthesis of 2,5-Dimethyl-2,5-hexanediol
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