Taylor J C, Hird S J, Sykes M D, Startin J R
Central Science Laboratory, Sand Hutton, York YO41 1LZ, UK.
Food Addit Contam. 2004 Jun;21(6):572-7. doi: 10.1080/02652030410001677763.
A simple, sensitive and reliable liquid chromatography-mass spectrometry method with direct injection of diluted samples is reported for the determination of propamocarb residues in wine. Red and white wines were diluted 40- and 20-fold, respectively, using water. Liquid chromatography was performed with a mobile-phase gradient and detection was by electrospray mass spectrometry in a positive ionization mode. Propamocarb was detected as the protonated molecular species at m/z 189. Using matrix-matched calibrant solutions, a calibrated range equivalent to 0.05-2.0 mg kg(-1) in red and white wines and limits of detection of 0.025 mg kg(-1) for white wine and of 0.05 mg kg(-1) for red wine (0.00125 microg ml(-1) of sample solution injected) were readily achievable. Recovery of propamocarb hydrochloride from wine spiked before dilution was in the range 91-115%. The chromatograms were free of isobaric interferences. In a small wine survey (72 samples), no residues of propamocarb were detected above 0.1 mg kg(-1).
报道了一种简单、灵敏且可靠的液相色谱-质谱法,可直接进样稀释后的样品来测定葡萄酒中的霜霉威残留量。红葡萄酒和白葡萄酒分别用水稀释40倍和20倍。液相色谱采用流动相梯度洗脱,检测采用电喷雾质谱的正离子模式。霜霉威以质荷比为189的质子化分子形式被检测到。使用基质匹配校准溶液,在红葡萄酒和白葡萄酒中可轻松实现相当于0.05 - 2.0 mg kg⁻¹的校准范围,白葡萄酒的检测限为0.025 mg kg⁻¹,红葡萄酒的检测限为0.05 mg kg⁻¹(进样0.00125 μg ml⁻¹的样品溶液)。稀释前加标的葡萄酒中盐酸霜霉威的回收率在91% - 115%范围内。色谱图中没有等压干扰。在一项小型葡萄酒调查(72个样品)中,未检测到霜霉威残留量超过0.1 mg kg⁻¹。