Identification of the impurities in chloroephedrine samples by HPLC-IT/TOF-MS and preparation of chloroephedrine standard

ABSTRACT

The identification of relevant impurities in the precursor chloroephedrine of the illegal drug methamphetamine will help for regulating this illegal drug and finding its sources. An efficient and effective method for qualitatively analysing samples of the drug was developed using high-performance liquid chromatography-hybrid ion trap/time-of-flight mass spectrometry (HPLC-IT/TOF MS). The chloroephedrine fragmentation pathway was proposed using HPLC-MSⁿ. Two impurities (1R, 2S)-β-chloro-methamphetamine and N-(1-phenyl-allyl)-β-chloro-methamphetamine in chloroephedrine samples were identified by the optimized HPLC-IT/TOF-MS. The synthetic route of the chloroephedrine samples was proposed by the analysis of these impurities. The established method would make it easy to identify impurities and find the source of this illegal drug. In addition, a method for the preparation of a chloroephedrine reference standard from actual samples was developed using preparative HPLC. The purity of the obtained standards was 99.51%.

KEYWORDS:

• High performance liquid chromatography-hybrid ion trap/time-of-flight mass spectrometry
• impurity identification
• chloroephedrine
• reference standards

Disclosure statement

No potential conflict of interest was reported by the authors.

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Funding

This work was supported by the National Natural Science Foundation of China under Grant No. 81671411; Special Fundamental Research Fund for the Central Public Scientific Research Institutes under Grant No. 562019Y-6671; the Fundamental Research Funds for the Central Universities under Grant XK1802-6; the Science and Technology Program of China Administration of Quality Supervision, Inspection and Quarantine under Grant 2017QK108; and the Chinese Central Level Public Welfare Scientific Research Institutes Foundation for Basic Research & Development under Grant 562016Y-5284.