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针对干果果肉基质含水量低、含糖量较高等特点,建立了改进的分散固相萃取结合超高效液相色谱-质谱/质谱法(UPLC-MS/MS)测定干果果肉培育过程中可能使用的56种农药残留量。样品经水浸润,以0.1%甲酸-乙腈提取,改进的分散固相萃取法(PSA)净化,液相色谱-质谱/质谱法检测,基质匹配标准曲线外标法定量。56种农药在10~500μg/L范围内线性关系良好,相关系数均大于0.990,在5,10和50μg/kg添加水平下56种农药回收率范围为60.4%~127.9%;相对标准偏差在1.1%~20%(n=6)之间;检出限和定量限分别为0.1~1.0μg/kg和0.3~3.1μg/kg。方法适合于干果果肉中56种农残检测。
Aiming at the low water content and higher sugar content of dried fruit pulp, an improved dispersive solid-phase extraction coupled with UPLC-MS / MS was developed to determine the possible use of dried fruit during pulp culture 56 kinds of pesticide residues. Samples were infiltrated with water, extracted with 0.1% formic acid - acetonitrile, modified by disperse solid - phase extraction (PSA), liquid chromatography - mass spectrometry / mass spectrometry, and matrix matching standard curve. The correlation coefficients of all 56 pesticides in the range of 10 ~ 500 μg / L were all above 0.990. The recoveries of 56 pesticides ranged from 60.4% to 127.9% at 5, 10 and 50 μg / kg levels with relative standard deviations of 1.1 % ~ 20% (n = 6). The limits of detection and quantification were 0.1 ~ 1.0μg / kg and 0.3 ~ 3.1μg / kg, respectively. The method is suitable for detecting 56 kinds of pesticide residues in dried fruit pulp.