title: Rapid quantification of iridoid glycosides analogues in the formulated Chinese medicine Longdan Xiegan Decoction using high-performance liquid chromatography coupled with mass spectrometry [corrected].
abstract: Longdan Xiegan Decoction (LXD) is a formulated preparation composed of 10 ingredient herbs, with iridoids as the main bioactive components. In this study, a rapid, simple and reliable method of simultaneous determination of four iridoid glycosides in LXD using high-performance liquid chromatography (HPLC) coupled with electrospray ionization mass spectrometry (MS) was first developed and validated. The four iridoid glycosides references were isolated from LXD extract and purified using a preparative HPLC chromatography. The sample preparation for quantification comprised of a simple ultrasonic extraction and the satisfactory chromatographic separation of the four structurally similar iridoid glycosides was effected in less than three minutes on a CAPCELL PAK C(18) MGII column (3 microm, 100 mm x 2.0 mm), using an elution system of 10% methanol and their concentrations in different batches of LXD and ingredient herbs were simultaneously determined by HPLC-MS/MS using a multiple reaction monitoring (MRM) mode. The method was validated with respect to the overall intra- and inter-day variation (RSD less than 8%) and the limits of quantification for the four iridoid glycosides were 35, 20, 37 and 33 ng/mL, respectively.
authors.affiliation: Key Laboratory of Standardization of Chinese Medicines of Ministry of Education, Shanghai University of Traditional Chinese Medicine, 1200 Cailun Road, Zhangjiang Hi-tech Park, Shanghai 201203, China.
authors.forename: Li
authors.initials: L
authors.lastname: Yang
authors.forename: Yun
authors.initials: Y
authors.lastname: Wang
authors.forename: Longxing
authors.initials: L
authors.lastname: Wang
authors.forename: Hongbin
authors.initials: H
authors.lastname: Xiao
authors.forename: Zhengtao
authors.initials: Z
authors.lastname: Wang
authors.forename: Zhibi
authors.initials: Z
authors.lastname: Hu
mesh_terms: D002851:Chromatography, High Pressure Liquid; D004304:Dosage Forms; D004365:Drugs, Chinese Herbal / Q000737:chemistry*; D006027:Glycosides / Q000032:analysis* / Q000737:chemistry; D039823:Iridoids / Q000032:analysis* / Q000737:chemistry; D016018:Least-Squares Analysis; D013058:Mass Spectrometry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
chemical_list: D004304:Dosage Forms; D004365:Drugs, Chinese Herbal; D006027:Glycosides; D039823:Iridoids; C526720:longdan xiegan decoction