Simultaneous analysis of kasugamycin and validamycin-A in fruits and vegetables using liquid chromatography-tandem mass spectrometry and consecutive solid-phase extraction. Issue 4 (12th January 2017)

• Record Type: Journal Article
• Authors: Wang, Chenchen; Li, Honge; Wang, Ni; Li, Huidong; Fang, Liping; Dong, Zhan; Du, Hongxia; Guan, Shuai; Zhu, Qian; Chen, Zilei; Yang, Guosheng
• Is Part Of: Analytical methods. Volume 9:Issue 4(2017)
• Page Start: 634
• Page End: 642
• Publication Date: 2017-01-12
• Subjects: Chemistry, Analytic -- Periodicals; Analytical biochemistry -- Periodicals; Chemical laboratories -- Standards -- Periodicals; 543.1905
• DOI: 10.1039/c6ay02921c
• Languages: English
• ISSNs: 1759-9660

Abstract

Abstract : A method based on a ReproSil 100 C18 column without any ion pairs or buffer additives is proposed for the determination of polar aminoglycosides. Abstract : A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for simultaneous determination of two hydrophilic aminoglycosides, kasugamycin and validamycin-A, in a variety of matrices (apples, cabbage, cucumbers, lettuce, tomatoes, and eggplant) has been developed. The proposed method provides sufficient sensitivity and excellent chromatographic performance using a special ReproSil 100 C18 column with 0.1% formic acid as the mobile phase additive. Accurate mass information for both analytes was obtained based on time-of-flight (TOF) mass spectrometry. The methanol/water (70 : 30, v/v) with pH adjusted to 5.5 was selected as the extraction solvent. The combination of hydrophilic–hydrophobic-balanced (HLB) cartridges with strong cation exchange SCX cartridges was used to purify the extracts with strongly polar compounds and satisfactory results were obtained. The consecutive solid-phase extraction minimized signal suppression/enhancement which led to matrix effects in the range of −12.6 to 6.11% only. Recovery experiments were performed for both compounds at three levels (50, 100, and 500 μg kg −1 ) in six different matrices and yielded good recoveries ranging from 81.7% to 108% with relative standard deviation values below 13%. The limits of quantification (LOQs) for kasugamycin and validamycin-A were 4.1 μg kg −1 and 1.0 μg kg −1, respectively.