摘要
【目的】为了测定浆果类水果(蓝莓、树莓、草莓及车厘子)中5-硝基对甲氧基苯酚钠(Sodium 5-nitroguaiacolate, 5NG)和对硝基苯酚钠(Sodium para-nitrophenolate, SD2)残留量,建立了快速测定5NG和SD2的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。【方法】样品用乙腈提取,无需富集浓缩等特殊净化步骤,以CAPCELL PKA-C18色谱柱分离,采用电喷雾(ESI~-)-多反应监测模式(MRM)检测,基质匹配标准溶液外标法定量。【结果】在0.02~2.00 mg/kg范围内,5NG和SD2的质量浓度与对应的峰面积间线性关系良好,相关系数均大于0.9968。5-硝基对甲氧基苯酚钠和对硝基苯酚钠在浆果类水果(蓝莓、树莓、草莓及车厘子)中的检出限(LOD)别为0.28~0.73μg/kg,定量限(LOQ)为0.93~2.43μg/kg。在4个添加水平下,样品添加回收试验的平均回收率为91.75%~112.67%,相对标准偏差为1.07%~5.76%(n=6)。【结论】该方法简单快捷,灵敏度高,定量准确,可用于同时检测蓝莓、树莓、草莓及车厘子中5NG和SD2的残留量。
【Objective】 In order to determine the 5-nitroguaiacolate(5 NG) and sodium para-nitrophenolate residues(SD2) in berries(blueberry, raspberry, strawberry and cherry), a rapid method for analyzing 5 NG and SD2 by ultra-high performance liquid chromatography-electrospray ionization-tandem mass spectrometry(UPLC-ESI-MS/MS) was developed. 【Method】 The sample was extracted with acetonitrile, and no moreclean-up procedures were needed.Successful separation and detection were achieved on a CAPCELL PKA-C18 column and multiple reaction monitoring(MRM) in negative electrospray ionization(ESI~-) mode was used. 【Result】 Quantification was performed by peak area external standard methods using matrix-matched calibration curves, which were linear in the range of 0.02-2.00 mg/kg with good linear relationships.The correlation coefficients were all above 0.9968. The limits of detection(LOD) and limits of quantification(LOQ)for 5 NG and SD2 were 0.28-0.73 and 0.93-2.43 μg/kg, respectively.At four spiked levels, the average recoveries ranged from 91.75 % to 112.67 %, and the relative standard deviation(n=6) was in the range of 1.07 %-5.76 %. 【Conclusion】 The method was quick,easy, sensitive, accurate and could be applied in the determination of 5 NG and SD2 residues in berries(blueberry, raspberry, strawberry and cherry).
引文
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