PMID- 34768158
OWN - NLM
STAT- MEDLINE
DCOM- 20211206
LR  - 20211214
IS  - 1873-264X (Electronic)
IS  - 0731-7085 (Linking)
VI  - 208
DP  - 2022 Jan 20
TI  - Separation of chiral and achiral impurities in paroxetine hydrochloride in a 
      single run using supercritical fluid chromatography with a polysaccharide 
      stationary phase.
PG  - 114458
LID - S0731-7085(21)00569-0 [pii]
LID - 10.1016/j.jpba.2021.114458 [doi]
AB  - Separating paroxetine hydrochloride and its impurities using conventional 
      reversed-phase liquid chromatography (RPLC) is challenging due to their highly 
      similar structures. In the present study, a rapid, simple, sensitive and 
      environmentally friendly method was developed for the determination of chiral and 
      achiral impurities in raw materials of paroxetine hydrochloride using chiral 
      supercritical fluid chromatography (SFC). The impacts of chiral stationary phases 
      (CSPs), mobile phases, column temperature and back pressure on the retention and 
      separation of analytes were comprehensively evaluated. After method optimization, 
      a satisfying result was obtained on a cellulose 
      tris-(3-chloro-4-methylphenylcarbamate) stationary phase in 4.0 min using 70% 
      CO(2) and 20 mM ammonium acetate in 30% methanol as the mobile phase. Molecular 
      docking was further performed to understand the interactions between the analytes 
      and CSP. The results suggested that hydrogen bonding and pi-pi interactions were 
      the dominant interactions. The affinity given by the software was in good 
      agreement with the elution order and free energy ( big up tri, openG) values obtained from van't 
      Hoff equations. The results of molecular docking also provide insights into the 
      different retentions of N-methylparoxetine at different temperatures. The results 
      of method validation revealed that the method was sensitive with a limit of 
      detection of approximately 0.05 mug.mL(-1) (corresponding to approximately 0.005% 
      paroxetine hydrochloride in the sample solution). The relative standard 
      deviations (RSDs) of precision and intra-assay precision were all less than 2.0%, 
      and the recoveries of the method were 93.8~105.3% with RSDs less than 3.0%. The 
      chiral and achiral RPLC methods included in the Chinese pharmacopoeia and the SFC 
      method proposed in this study were simultaneously used to determine the impurity 
      content in the raw materials of paroxetine hydrochloride. The results showed that 
      impurities that cannot be detected by the reference method can be accurately 
      quantified using the SFC method. In addition, the SFC method has advantages in 
      terms of throughput, analysis cost and simplicity. This study can provide a 
      reference for further research of impurities in paroxetine hydrochloride and 
      promote the application of chiral SFC in the rapid separation of structurally 
      similar compounds.
CI  - Copyright (c) 2021 Elsevier B.V. All rights reserved.
FAU - Qiu, Xiaodan
AU  - Qiu X
AD  - Institute of Medicinal Biotechnology, Peking Union Medical College & Chinese 
      Academy of Medical Sciences, No.1, Tian Tan Xi Li, 100050 Beijing, PR China.
FAU - Liu, Yitong
AU  - Liu Y
AD  - Institute of Medicinal Biotechnology, Peking Union Medical College & Chinese 
      Academy of Medical Sciences, No.1, Tian Tan Xi Li, 100050 Beijing, PR China.
FAU - Zhao, Ting
AU  - Zhao T
AD  - Institute of Medicinal Biotechnology, Peking Union Medical College & Chinese 
      Academy of Medical Sciences, No.1, Tian Tan Xi Li, 100050 Beijing, PR China.
FAU - Zuo, Limin
AU  - Zuo L
AD  - Institute of Medicinal Biotechnology, Peking Union Medical College & Chinese 
      Academy of Medical Sciences, No.1, Tian Tan Xi Li, 100050 Beijing, PR China.
FAU - Ma, Xun
AU  - Ma X
AD  - China National Institutes for Food and Drug Control, No. 2, Tian Tan Xi Li, 
      100050 Beijing, PR China. Electronic address: maxun@nifdc.org.cn.
FAU - Shan, Guangzhi
AU  - Shan G
AD  - Institute of Medicinal Biotechnology, Peking Union Medical College & Chinese 
      Academy of Medical Sciences, No.1, Tian Tan Xi Li, 100050 Beijing, PR China. 
      Electronic address: shanguangzhi@imb.pumc.edu.cn.
LA  - eng
PT  - Journal Article
DEP - 20211102
PL  - England
TA  - J Pharm Biomed Anal
JT  - Journal of pharmaceutical and biomedical analysis
JID - 8309336
RN  - 0 (Polysaccharides)
RN  - 41VRH5220H (Paroxetine)
SB  - IM
MH  - *Chromatography, Supercritical Fluid
MH  - Molecular Docking Simulation
MH  - Paroxetine
MH  - Polysaccharides
MH  - Stereoisomerism
OTO - NOTNLM
OT  - Impurities
OT  - Molecular docking
OT  - Paroxetine hydrochloride
OT  - Supercritical fluid chromatography
COIS- Declaration of Competing Interest The authors declare that they have no known 
      competing financial interests or personal relationships that could have appeared 
      to influence the work reported in this paper.
EDAT- 2021/11/13 06:00
MHDA- 2021/12/15 06:00
CRDT- 2021/11/12 20:28
PHST- 2021/08/11 00:00 [received]
PHST- 2021/10/29 00:00 [revised]
PHST- 2021/10/30 00:00 [accepted]
PHST- 2021/11/13 06:00 [pubmed]
PHST- 2021/12/15 06:00 [medline]
PHST- 2021/11/12 20:28 [entrez]
AID - S0731-7085(21)00569-0 [pii]
AID - 10.1016/j.jpba.2021.114458 [doi]
PST - ppublish
SO  - J Pharm Biomed Anal. 2022 Jan 20;208:114458. doi: 10.1016/j.jpba.2021.114458. 
      Epub 2021 Nov 2.