title: Determination of validamycin A in agricultural food samples by solid-phase extraction combined with liquid chromatography-atmospheric pressure chemical ionisation-tandem mass spectrometry.
abstract: For the first time, a rapid, sensitive and accurate liquid chromatography-atmospheric pressure chemical ionisation-tandem mass spectrometry (LC-APCI-MS/MS) method was developed for determination of validamycin A in agricultural food samples (rice, agaric, almond, cabbage, green onion, carrot, tomato, cucumber and spinach). The validamycin A residue was extracted with methanol-water (9/1, v/v) or methanol by vortex, and a HLB solid-phase extraction cartridge was used for cleaning up the extracts. LC-APCI-MS/MS data acquisition was carried out in multiple reaction monitoring (MRM) mode. A series of matrix-matched calibration solutions ranging from 2.5 to 50ngmL(-1) were used to record calibration curve. The limit of quantification (LOQ) was 10μgkg(-1). The average recoveries, measured at three concentrations levels (10.0, 50.0, 100.0μgkg(-1)) were in the range 83.5-109.6%. The proposed method offers the best sensitivity and specificity for the routine analysis of validamycin A in agricultural food samples.
authors.affiliation: Shanghai Entry-Exit Inspection and Quarantine Bureau of P.R.C, Shanghai 200135, China.
authors.forename: Chuanxian
authors.initials: C
authors.lastname: Wang
authors.affiliation: Xiamen Entry-Exit Inspection and Quarantine Bureau of P.R.C, Xiamen 361026, China.
authors.forename: Zhigang
authors.initials: Z
authors.lastname: Zhang
authors.affiliation: College of Chemistry and Materials Engineering, Wenzhou University, Wenzhou 325035, China. Electronic address: shenyan@wzu.edu.cn.
authors.forename: Yan
authors.initials: Y
authors.lastname: Shen
authors.affiliation: Shanghai Entry-Exit Inspection and Quarantine Bureau of P.R.C, Shanghai 200135, China.
authors.forename: Zhengan
authors.initials: Z
authors.lastname: Tian
authors.affiliation: Xiamen Entry-Exit Inspection and Quarantine Bureau of P.R.C, Xiamen 361026, China.
authors.forename: Dunming
authors.initials: D
authors.lastname: Xu
authors.affiliation: Wenzhou Entry-Exit Inspection and Quarantine Bureau of P.R.C, Wenzhou 325027, China. Electronic address: chaohan96@hotmail.com.
authors.forename: Chao
authors.initials: C
authors.lastname: Han
mesh_terms: D001274:Atmospheric Pressure; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D018556:Crops, Agricultural / Q000737:chemistry*; D007294:Inositol / Q000031:analogs & derivatives* / Q000032:analysis / Q000302:isolation & purification; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: C030790:validamycin A; D007294:Inositol
keywords: Agricultural food samples; LC–APCI–MS/MS; Solid-phase extraction; Validamycin A