title: Identification, Characterization, Synthesis and Quantification of Related Impurities of Liguzinediol.
abstract: An HPLC method was employed to create an impurity profile for liguzinediol as an active pharmaceutical ingredient (API), which resulted in the identification of two related impurities. Therefore, in order to improve the quality control of the liguzinediol-API, we identified and then developed a method for quantifying the two impurities (impurity-1 and impurity-2) by LC-TOF-MS-MS and then chemically synthesized them for further studies. Based on spectral data from IR, MS, (1)H and (13)C NMR, the structures of impurity-1 and impurity-2 were characterized as 2-hydroxymethyl-3,6-dimethylpyrazine and 2-hydroxymethyl-3,5,6-trimethylpyrazine, respectively. We further validated the method according to the International Conference on Harmonization guidelines to demonstrate the sensitivity, precision, linearity, accuracy and stability of the method described. In addition, the potential mechanisms underlying formation of impurity-1 and impurity-2 in the liguzinediol-API are discussed in detail.
authors: School of Pharmacy, Nanjing University of Chinese Medicine, Nanjing 210023, China.
authors: Dong
authors: D
authors: Cheng
authors: School of Pharmacy, Nanjing University of Chinese Medicine, Nanjing 210023, China.
authors: Ying
authors: Y
authors: Zhou
authors: School of Pharmacy, Nanjing University of Chinese Medicine, Nanjing 210023, China liwaii@126.com.
authors: Wei
authors: W
authors: Li
authors: School of Pharmacy, Nanjing University of Chinese Medicine, Nanjing 210023, China.
authors: Chen-Xiao
authors: CX
authors: Shan
authors: School of Pharmacy, Nanjing University of Chinese Medicine, Nanjing 210023, China.
authors: Chuan
authors: C
authors: Chai
authors: School of Pharmacy, Nanjing University of Chinese Medicine, Nanjing 210023, China.
authors: Xiao-Bing
authors: XB
authors: Cui
authors: School of Pharmacy, Nanjing University of Chinese Medicine, Nanjing 210023, China.
authors: Bi
authors: B
authors: Kang
authors: School of Pharmacy, Nanjing University of Chinese Medicine, Nanjing 210023, China.
authors: Tian-Lin
authors: TL
authors: Wang
authors: School of Pharmacy, Nanjing University of Chinese Medicine, Nanjing 210023, China.
authors: Hong-Mei
authors: HM
authors: Wen
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004340:Drug Contamination; D004355:Drug Stability; D016014:Linear Models; D011719:Pyrazines / Q000032:analysis* / Q000737:chemistry*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D059629:Signal-To-Noise Ratio
chemical_list: C572935:2,5-dihydroxymethyl-3,6-dimethylpyrazine; D011719:Pyrazines