QuEChERS Sample Preparation for Determination of Steroids Adulterated in Herbal Pills by High Performance Liquid Chromatography

Abstract

Adulterations with synthetic steroids are common problems of herbal medicines
and this can potentially cause serious adverse effects to consumers. It is important to determine
the presence of synthetic steroids and effective analytical method is therefore critically important.
The objective of this study was to develop the QuEChERS sample preparation for high
performance liquid chromatography (HPLC) determination of two steroids, prednisolone and
dexamethasone, adulterated in herbal pills. In QuEChERS procedures, a 0.5 g of sample was
extracted with acetonitrile (3.0 ml) and then anhydrous magnesium sulfate (0.5 g) and sodium
chloride (0.125 g). Then simple cleanup was performed by dispersive–solid phase extraction
using PSA sorbents as well as magnesium sulfate for the removal of residual water. Using
HPLC separation, the QuEChERS extraction gave the limits of detection of 0.36 and 0.6 mg/
kg, respectively. Blank sample of herbal pills were spiked with prednisolone and dexamethasone
at two levels of 10 and 50 mg/kg, acceptable recoveries of 82–97% were obtained with
relative standard deviation less than 5%. The technique was simple, convenient, rapid, and
consumed less chemical and organic solvent. It was suitable to analyse prednisolone and
dexamethasone adulterated in herbal medicines for the benefit of consumer protection.