Premium
Simultaneous determination of diethylene glycol and propylene glycol in pharmaceutical products by HPLC after precolumn derivatization with p ‐toluenesulfonyl isocyanate
Author(s) -
Zhou Tao,
Zhang Haiying,
Duan Gengli
Publication year - 2007
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200700097
Subject(s) - diethylene glycol , derivatization , chromatography , chemistry , isocyanate , high performance liquid chromatography , phosphoric acid , reagent , detection limit , calibration curve , triethylene glycol , ethylene glycol , organic chemistry , polyurethane
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 μL, 20% in ACN v/v) was added to 100 μL of the sample, and then 10 μL 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°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 μg/mL ( r 2 = 0.9999) and from 0.071 to 21.3 μg/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.