PMID- 21708383
OWN - NLM
STAT- MEDLINE
DCOM- 20111011
LR  - 20131121
IS  - 1873-3778 (Electronic)
IS  - 0021-9673 (Linking)
VI  - 1218
IP  - 35
DP  - 2011 Sep 2
TI  - Method development and validation for optimised separation of salicylic, acetyl 
      salicylic and ascorbic acid in pharmaceutical formulations by hydrophilic 
      interaction chromatography and response surface methodology.
PG  - 5995-6003
LID - 10.1016/j.chroma.2011.06.009 [doi]
AB  - This paper introduces a design of experiments (DOE) approach for method 
      optimisation in hydrophilic interaction chromatography (HILIC). An optimisation 
      strategy for the separation of acetylsalicylic acid, its major impurity salicylic 
      acid and ascorbic acid in pharmaceutical formulations by HILIC is presented, with 
      the aid of response surface methodology (RSM) and Derringer's desirability 
      function. A Box-Behnken experimental design was used to build the mathematical 
      models and then to choose the significant parameters for the optimisation by 
      simultaneously taking both resolution and retention time as the responses. The 
      refined model had a satisfactory coefficient (R(2)>0.92, n=27). The four 
      independent variables studied simultaneously were: acetonitrile content of the 
      mobile phase, pH and concentration of buffer and column temperature each at three 
      levels. Of these, the concentration of buffer and its cross-product with pH had a 
      significant, positive influence on all studied responses. For the test compounds, 
      the best separation conditions were: acetonitrile/22 mM ammonium acetate, pH 4.4 
      (82:18, v/v) as the mobile phase and column temperature of 28 degrees C. The methodology 
      also captured the interaction between variables which enabled exploration of the 
      retention mechanism involved. It would be inferred that the retention is governed 
      by a compromise between hydrophilic partitioning and ionic interaction. The 
      optimised method was further validated according to the ICH guidelines with 
      respect to linearity and range, precision, accuracy, specificity and sensitivity. 
      The robustness of the method was also determined and confirmed by overlying 
      counter plots of responses which were derived from the experimental design 
      utilised for method optimisation.
CI  - Copyright (c) 2011 Elsevier B.V. All rights reserved.
FAU - Hatambeygi, Nader
AU  - Hatambeygi N
AD  - Kimiafaam Pharmaceutical Co., Tehran 11458, Iran.
FAU - Abedi, Ghazaleh
AU  - Abedi G
FAU - Talebi, Mohammad
AU  - Talebi M
LA  - eng
PT  - Journal Article
DEP - 20110612
PL  - Netherlands
TA  - J Chromatogr A
JT  - Journal of chromatography. A
JID - 9318488
RN  - 0 (Acetates)
RN  - 0 (Acetonitriles)
RN  - 0 (Tablets)
RN  - O414PZ4LPZ (Salicylic Acid)
RN  - PQ6CK8PD0R (Ascorbic Acid)
RN  - R16CO5Y76E (Aspirin)
RN  - RRE756S6Q2 (ammonium acetate)
RN  - Z072SB282N (acetonitrile)
SB  - IM
MH  - Acetates/chemistry
MH  - Acetonitriles/chemistry
MH  - Analysis of Variance
MH  - Ascorbic Acid/analysis/*isolation & purification
MH  - Aspirin/analysis/*isolation & purification
MH  - Chromatography, Liquid/*methods
MH  - Drug Contamination
MH  - Hydrogen-Ion Concentration
MH  - *Hydrophobic and Hydrophilic Interactions
MH  - Least-Squares Analysis
MH  - Models, Chemical
MH  - Reproducibility of Results
MH  - Salicylic Acid/analysis/*isolation & purification
MH  - Sensitivity and Specificity
MH  - Tablets/chemistry
MH  - Temperature
EDAT- 2011/06/29 06:00
MHDA- 2011/10/12 06:00
CRDT- 2011/06/29 06:00
PHST- 2010/04/20 00:00 [received]
PHST- 2011/05/31 00:00 [revised]
PHST- 2011/06/02 00:00 [accepted]
PHST- 2011/06/29 06:00 [entrez]
PHST- 2011/06/29 06:00 [pubmed]
PHST- 2011/10/12 06:00 [medline]
AID - S0021-9673(11)00805-3 [pii]
AID - 10.1016/j.chroma.2011.06.009 [doi]
PST - ppublish
SO  - J Chromatogr A. 2011 Sep 2;1218(35):5995-6003. doi: 10.1016/j.chroma.2011.06.009. 
      Epub 2011 Jun 12.