A rapid tandem mass spectrometric assay for determination of ursolic acid: Application to analysis of ursolic acid in four species of Staphylea L. and leaves of Staphylea pinnata L. gathered during ontogenesis

• Published in: Chromatographia Vol. 63; no. 3-4; pp. 117 - 122
• Main Authors: LACIKOVA, L, ABDEL-HAMID, M. E, NOVOTNY, L, MASTEROVA, I, GRANCAI, D
• Format: Journal Article
• Language: English
• Published: Oxford Springer 01.02.2006; Springer Nature B.V
• Subjects: Acids; Biological and medical sciences; Cycle time; Flow injection analysis; Formic acid; General pharmacology; Medical sciences; Pharmacognosy. Homeopathy. Health food; Pharmacology. Drug treatments; Spectrometry; Pentacyclic compound; Validation; Terpenoid; Liquid chromatography-tandem mass spectrometry Flow injection analysis Skiphylea pinnata; Chemical analysis; Coupled method; Pharmacognosy; HPLC chromatography; Plant leaf; Solvent extraction; Staphylea holocarpa; Medicinal plant; Sample preparation; Staphyleaceae; Staphylea elegans; Dicotyledones; Mass spectrometry MS/MS; Angiospermae; Plant origin; Triterpene; Spermatophyta; and Staphylea colchica; Quantitative analysis; Flow injection
• ISSN: 0009-5893; 1612-1112
• DOI: 10.1365/s10337-006-0724-y

Plant extracts of Staphylea L. exhibit a number of biological activities which are presumably attributed to ursolic acid. A rapid and specific tandem mass spectrometric (MS-MS) assay for the quantification of ursolic acid in the leaves of four species of Staphylea L. (Bladdernut) and in the leaves of S. pinnata L. during ontogenesis, was developed and validated. The samples were analyzed by flow injection analysis without chromatographic separation using a transport liquid of methanol/water/formic acid (80:20:0.1 v/v/v) at a flow-rate of 0.2 mL min−1. The run cycle time was ~2-3 min injection-to-injection. Quantification was achieved using multiple reaction monitoring at MRM transition m/z 439 > 203. Calibration curves were linear over the concentration range of 2–20 µg mL−1 with a lower limit of quantification of 2 µg mL−1 (1.8 ± 0.297, RSD: 0.165). Validation data showed that the RSD% values were in the range of 1.8 to 6.8%, whereas the % DEVs ranged from −18 to −2% indicating reasonable and acceptable precision and accuracy, respectively. A recovery percent of 106.8 ± 10.3 of ursolic acid from spiked extracts samples, indicated the specificity and reliability of tandem mass procedure for determination of ursolic acid in the plant extracts. The derived data of sample analysis showed different contents of ursolic acid among various Staphylea species. The highest content of ursolic acid was found in the leaves extract of S. pinnata L. Additionally, the highest amount of ursolic acid accumulated in the leaves of S. pinnata L. was in the August /September period of the year. Smaller amounts of ursolic acid were found in samples collected before and after that time. The results obtained serve as a justification of determining the most appropriate time for collecting plant material as a source of ursolic acid.