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Food Chem. 2015 Feb 15;169:150-5. doi: 10.1016/j.foodchem.2014.07.145. Epub 2014 Aug 7.

Determination of validamycin A in agricultural food samples by solid-phase extraction combined with liquid chromatography-atmospheric pressure chemical ionisation-tandem mass spectrometry.

Author information

1
Shanghai Entry-Exit Inspection and Quarantine Bureau of P.R.C, Shanghai 200135, China.
2
Xiamen Entry-Exit Inspection and Quarantine Bureau of P.R.C, Xiamen 361026, China.
3
College of Chemistry and Materials Engineering, Wenzhou University, Wenzhou 325035, China. Electronic address: shenyan@wzu.edu.cn.
4
Wenzhou Entry-Exit Inspection and Quarantine Bureau of P.R.C, Wenzhou 325027, China. Electronic address: chaohan96@hotmail.com.

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.

KEYWORDS:

Agricultural food samples; LC–APCI–MS/MS; Solid-phase extraction; Validamycin A

PMID:
25236210
DOI:
10.1016/j.foodchem.2014.07.145
[Indexed for MEDLINE]

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