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采用将内标溶于油脂中的方法对样品前处理,冷冻高速离心去除油脂及杂质干扰,应用高效液相色谱柱进行分离,采用电喷雾(ESI),以负离子检测方式进行质谱分析,同位素内标法定量,建立了液相色谱-质谱(LC-MS-MS)法检测ARA&DHA油脂中壬基酚(NP)含量的方法。实验结果表明,壬基酚质量浓度在5μg/kg~500μg/kg范围内与色谱峰面积呈良好的线性关系,相关系数R~2=0.9998,检出限为0.3μg/kg。在3个添加水平下,样品的加标回收率为96.9%~105.2%,相对标准偏差(RSD)在2.9%~7.3%之间(n=6)。该方法的建立为ARA&DHA油脂中壬基酚的检测提供了一种前处理简便、选择性好、灵敏度高的检测方法。
The internal standard was dissolved in oil for sample pretreatment, frozen high-speed centrifugation to remove oil and impurities interference, the use of high performance liquid chromatography column separation, the use of electrospray (ESI), negative ion detection mass spectrometry, isotope The method of LC-MS-MS was established for the determination of nonylphenol (NP) in ARA & DHA oil. The experimental results showed that the concentration of nonylphenol in the range of 5μg / kg ~ 500μg / kg and the chromatographic peak area showed a good linear relationship, the correlation coefficient R ~ 2 = 0.9998, the detection limit of 0.3μg / kg. The recoveries of spiked samples ranged from 96.9% to 105.2% with relative standard deviations (RSDs) between 2.9% and 7.3% (n = 6) at the three addition levels. The establishment of this method provides a convenient, selective, and sensitive detection method for the detection of nonylphenol in ARA & DHA oils.