Document Detail

Simultaneous determination of diethylene glycol and propylene glycol in pharmaceutical products by HPLC after precolumn derivatization with p-toluenesulfonyl isocyanate.
MedLine Citation:
PMID:  17880028     Owner:  NLM     Status:  MEDLINE    
A simple and reliable HPLC method was developed for the simultaneous quantitative analysis of diethylene glycol (DEG) and propylene glycol (PG) in pharmaceutical products by precolumn derivatization. The derivatization reagent p-toluenesulfonyl isocyanate (TSIC, 10 microL, 20% in ACN v/v) was added to 100 microL of the sample, and then 10 muL of water was added. The resulting derivatives were separated using a C(18)analytical column and a mobile phase composed of 0.01 M KH(2)PO(4)buffer (adjusted to pH 2.5 with phosphoric acid) and ACN (47:53 v/v) at 1 mL/min and 25 degrees C. For detection, UV light at 227 nm was used. The derivatization conditions including reaction time, temperature, and concentration of TSIC were optimized. The calibration curves were linear from 0.062 to 18.6 microg/mL (r(2)= 0.9999) and from 0.071 to 21.3 microg/mL (r(2) = 0.9999) for DEG and PG, respectively. The RSD values of intra- and interday assays were all below 4% for DEG and PG. The proposed method was then successfully applied to analyze two Armillarisin A injection samples and two spiked syrup samples.
Tao Zhou; Haiying Zhang; Gengli Duan
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Publication Detail:
Type:  Journal Article    
Journal Detail:
Title:  Journal of separation science     Volume:  30     ISSN:  1615-9306     ISO Abbreviation:  J Sep Sci     Publication Date:  2007 Nov 
Date Detail:
Created Date:  2007-12-17     Completed Date:  2008-01-07     Revised Date:  -    
Medline Journal Info:
Nlm Unique ID:  101088554     Medline TA:  J Sep Sci     Country:  Germany    
Other Details:
Languages:  eng     Pagination:  2620-7     Citation Subset:  IM    
Department of Pharmaceutical Analysis, School of Pharmacy, Fudan University, Shanghai, PR China.
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MeSH Terms
Chromatography, High Pressure Liquid / methods*
Ethylene Glycols / analysis*
Isocyanates / chemistry*
Pharmaceutical Preparations / chemistry*
Propylene Glycol / analysis*
Reference Standards
Sensitivity and Specificity
Spectrophotometry, Ultraviolet
Tosyl Compounds / chemistry*
Reg. No./Substance:
0/Ethylene Glycols; 0/Isocyanates; 0/Pharmaceutical Preparations; 0/Tosyl Compounds; 111-46-6/diethylene glycol; 57-55-6/Propylene Glycol

From MEDLINE®/PubMed®, a database of the U.S. National Library of Medicine

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