【求助】哪位用液质做过霜霉威啊？

Determination of propamocarb in vegetables using polymer-based high-performance liquid chromatography coupled with electrospray mass spectrometry
Maurice Hiemstra, André de Kok
Journal of Chromatography A Volume 972, Issue 2, 4 October 2002, Pages 231-239
Abstract
A method for the determination of propamocarb in vegetables with liquid chromatography–electrospray ionisation mass spectrometry ($$lc–ESI-MS) was developed. The performance of a polymer-based analytical $$lc column for the separation was investigated. Residues of propamocarb were extracted from the matrix with methanol. Subsequently, the extract was directly injected into the $$lc–MS system, without any additional concentration or cleanup procedures. Separation of propamocarb from the matrix components was achieved on a polymethacrylate-based analytical column. Propamocarb was concurrently detected with electrospray ionisation mass spectrometry in the selected ion monitoring mode and two-stage full scan MS application. Quantitation was done with matrix-matched calibration standards of propamocarb. Unambiguous confirmation was achieved by comparison of the full scan product ion mass spectrum of the chromatographic peak in the sample with the spectrum of a standard solution of propamocarb at the same retention time. The analytical performance of the method was validated for five relevant matrices, spiking propamocarb at fortification levels from 0.05 to 15.0 mg kg−1. This covers the range of maximum residue limits in agricultural commodities, stated in the Dutch national legislation. The mean recovery of propamocarb was better than 90% with a precision of less than 10% in both scanning applications. As could be concluded from the calibration curve and matrix background levels, observed in blank control samples, the estimated limit of detection was 25 μg kg−1 for the two-stage full scan MS application. The method has been applied in a survey of 285 samples of lettuce, radish, leek, and cabbage for the presence of residues of propamocarb. In 50% of the samples analysed, a residue of propamocarb was detected.

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