PMID- 35543467
OWN - NLM
STAT- MEDLINE
DCOM- 20221229
LR  - 20221229
IS  - 1944-7922 (Electronic)
IS  - 1060-3271 (Linking)
VI  - 105
IP  - 5
DP  - 2022 Sep 6
TI  - Application of Chemometry and Design of Experiments to Green HPTLC Method for 
      Synchronous Estimation of Multiple FDCs of Cilnidipine.
PG  - 1491-1501
LID - 10.1093/jaoacint/qsac056 [doi]
AB  - BACKGROUND: Numerous fixed-dose combinations (FDCs) of cilnidipine (CIL) with 
      chlorthalidone (CLT) and azilsartan medoxomil (AZL) are used for the treatment of 
      hypertension. Numerous reverse-phase high-pressure liquid chromatography 
      (RP-HPLC) and high-performance thin-layer chromatography (HPTLC) methods have 
      been reported in the literature for the estimation of FDCs of CIL. But no HPTLC 
      method has been reported yet for synchronous estimation of multiple FDCs of CIL 
      to save time, organic solvent, and cost of analysis. In the recent scenario of 
      green chemistry, the minimum usage of organic solvent in the development of the 
      chromatographic method is highly desirable for the safety of the environment and 
      analysts. OBJECTIVE: Hence, a robust and green HPTLC method has been developed 
      for the synchronous estimation of multiple FDCs of CIL using the analytical 
      quality by design (AQbD) approach. METHODS: The chemometric tool was applied for 
      the identification of the critical method variables (CMVs) and critical 
      analytical attributes (CAAs) for the HPTLC method development. The design of 
      experiments (DoE) was applied for the response surface analysis of identified 
      CMVs and CAAs using the Box-Behnken design. The analytical design space and 
      control strategy was framed for the lifecycle management of the HPTLC method. 
      RESULTS: The chromatographic separation was performed using silica gel G60 F254 
      as the stationary phase and toluene-ethyl acetate-methanol (6.5 + 2 + 1.5, v/v) 
      as the mobile phase. The method was validated as per the International Council 
      for Harmonization Q2 (R1) guideline. The developed method was applied for the 
      synchronous estimation of multiple FDCs of CIL, and results were found in 
      compliance with labeled claims. CONCLUSIONS: The developed HPTLC method can be 
      used as a green, economical, and rapid analytical tool for routine analysis and 
      quality control of multiple FDCs of CIL in the pharmaceutical industry. 
      HIGHLIGHTS: Development of a HPTLC method for synchronous estimation of multiple 
      FDCs of CIL using the AQbD approach based on principles of chemometry and DoE. 
      Application of the developed method for synchronous assay of multiple FDCs of CIL 
      to save time, cost, and solvent for analysis.
CI  - (c) The Author(s) 2022. Published by Oxford University Press on behalf of AOAC 
      INTERNATIONAL. All rights reserved. For permissions, please email: 
      journals.permissions@oup.com.
FAU - Prajapati, Pintu
AU  - Prajapati P
AUID- ORCID: 0000-0002-5282-2087
AD  - Maliba Pharmacy College, Maliba Campus, Department of Quality Assurance, 
      Bardoli-Mahuva Road, Tarsadi, Mahuva, Surat, 394 350 Gujarat, India.
FAU - Tailor, Pratik
AU  - Tailor P
AUID- ORCID: 0000-0001-7675-1458
AD  - Maliba Pharmacy College, Maliba Campus, Department of Quality Assurance, 
      Bardoli-Mahuva Road, Tarsadi, Mahuva, Surat, 394 350 Gujarat, India.
FAU - Shahi, Abhinandan
AU  - Shahi A
AUID- ORCID: 0000-0001-9648-5724
AD  - Maliba Pharmacy College, Maliba Campus, Department of Quality Assurance, 
      Bardoli-Mahuva Road, Tarsadi, Mahuva, Surat, 394 350 Gujarat, India.
FAU - Acharya, Aneri
AU  - Acharya A
AUID- ORCID: 0000-0003-0175-6697
AD  - Maliba Pharmacy College, Maliba Campus, Department of Quality Assurance, 
      Bardoli-Mahuva Road, Tarsadi, Mahuva, Surat, 394 350 Gujarat, India.
FAU - Shah, Shailesh
AU  - Shah S
AUID- ORCID: 0000-0002-1039-9882
AD  - Maliba Pharmacy College, Maliba Campus, Department of Quality Assurance, 
      Bardoli-Mahuva Road, Tarsadi, Mahuva, Surat, 394 350 Gujarat, India.
LA  - eng
PT  - Journal Article
PL  - England
TA  - J AOAC Int
JT  - Journal of AOAC International
JID - 9215446
RN  - 97T5AZ1JIP (cilnidipine)
RN  - 0 (Dihydropyridines)
RN  - 0 (Solvents)
SB  - IM
MH  - *Chemometrics
MH  - Chromatography, Thin Layer/methods
MH  - Dihydropyridines
MH  - Reproducibility of Results
MH  - Solvents
EDAT- 2022/05/12 06:00
MHDA- 2022/09/08 06:00
CRDT- 2022/05/11 08:34
PHST- 2022/02/04 00:00 [received]
PHST- 2022/03/23 00:00 [revised]
PHST- 2022/04/29 00:00 [accepted]
PHST- 2022/05/12 06:00 [pubmed]
PHST- 2022/09/08 06:00 [medline]
PHST- 2022/05/11 08:34 [entrez]
AID - 6584003 [pii]
AID - 10.1093/jaoacint/qsac056 [doi]
PST - ppublish
SO  - J AOAC Int. 2022 Sep 6;105(5):1491-1501. doi: 10.1093/jaoacint/qsac056.