Simultaneous determination of diethylene glycol and propylene glycol in pharmaceutical products by HPLC after precolumn derivatization with p‐toluenesulfonyl isocyanate

Abstract

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.

D‐Lactate production as a function of glucose metabolism in Saccharomyces cerevisiae

“…Media 1,2-propanediol was derivatized with p -toluenesulfonyl isocyanate and measured by HPLC according to the method of Zhou (Zhou, et al, 2007). …”

Determination of Propylene Glycol in Low Volume Plasma and Urine Samples of Neonates by LC with Photodiode Array Detection

“…Considering blood sampling constraints in neonates and frequently available only limited sampling volumes of plasma and urine, a bioanalytical method for measuring PG in low volume plasma and urine samples is needed to evaluate possible PG accumulation and the level of safe exposure in this specific high risk population. So far, for PG determination gas chromatographic (GC) methods [3,[15][16][17][18] and high performance liquid chromatographic (HPLC) methods combined with mass spectrometry (MS) [19] or ultraviolet detection [20,21] have been described. Derivatisation-free LC method with refractive index (RI) detection for PG determination was also described [22] but nowadays, the PG assay is typically performed by HPLC with precolumn derivatisation [19][20][21].…”

Detection of Diethylene Glycol in Glycerin and Propylene Glycol by using high performance thin layer chromatography HPTLC

“…USP, British, European pharmacopeias mentioned in monograph of Glycerin to Gas chromatography method for detection of Diethylene Glycol and Ethylene Glycol in Glycerin as raw material (14,15,16) . And there are many reference methods based on high-performance liquid chromatography HPLC (17,18,19,20) . World Health Organization (WHO) and Food and Drug Administration (FDA) had provided a method of thinlayer chromatography TLC (limit method), which were used to detect DEG in Glycerin, Propylene Glycol, and Sorbitol after spray the plate with permanganate solution or iodine.…”