Chromatography and Separation Research Unit, Department of Chemistry, Faculty of Science, Chulalongkorn University, Bangkok 10330, Thailand.
J Pharm Biomed Anal. 2011 Jul 15;55(5):1175-8. doi: 10.1016/j.jpba.2011.03.046. Epub 2011 Apr 8.
QuEChERS sample preparation was optimized using solvent extraction with acetonitrile and dispersive-solid phase extraction with primary and secondary amine sorbents, and validated for high-performance liquid chromatographic determination of nine steroids commonly used to adulterate herbal medicines: such as triamcinolone, prednisolone, hydrocortisone, methylprednisolone, betamethasone, dexamethasone, beclomethasone, fludrocortsone acetate and cortisone acetate. Satisfactory extraction recoveries of 91-113% for all nine steroids were obtained, along with an acceptable precision in extraction recoveries shown by R.S.D. of ≤4.6 and 3.2% for intraday and interday, respectively. The QuEChERS sample preparation developed here allows the reliable detection of adulterated steroids with the limits of detection in the range of 0.06-0.17ppm. Adulterated steroids in three out of six real commercial liquid herbal medicines were found, such as 1.6 and 8.8ppm dexamethasone and 0.43ppm prednisolone.
采用乙腈溶剂萃取和初级及次级胺吸附剂分散固相萃取对 QuEChERS 样品前处理进行优化，用于高效液相色谱法测定常用于掺假草药的九种甾体激素：曲安西龙、泼尼松龙、氢化可的松、甲泼尼龙、倍他米松、地塞米松、倍氯米松、醋酸氟氢可的松和醋酸可的松。所有九种甾体激素的提取回收率均为 91-113%，日内和日间提取回收率的精密度分别为 RSD≤4.6%和 3.2%，表明结果可接受。这里开发的 QuEChERS 样品前处理方法可可靠检测到掺杂的甾体激素，检出限在 0.06-0.17ppm 范围内。在六种实际商业液体草药制剂中的三种中发现了掺杂的甾体激素，如 1.6ppm 和 8.8ppm 的地塞米松以及 0.43ppm 的泼尼松龙。
