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目的应用气相色谱-质谱联用技术,建立食用油中17种邻苯二甲酸酯类物质的检测方法。方法样品加入内标物后经乙腈提取,4000 r/min离心5 min,吸取乙腈相经SILICA/PSA混合玻璃柱净化后,经过HP-5MS色谱柱程序升温分离,用气相色谱-质谱联用仪检测,选择离子模式测定,内标法定量。结果该方法最低检出浓度为0.1 mg/kg~0.5 mg/kg,在0.2μg/ml~2μg/ml范围内线性良好,r2为0.992~1.000,进行低、高2个浓度水平17种邻苯二甲酸酯同时添加,测定添加回收率,回收率范围为75.5%~118.8%,相对标准偏差为3.7%~13.9%。结论该方法灵敏度高,净化效果好、能够快速准确的测定食用油中17种邻苯二甲酸酯类物质。
Objective To establish a method for the determination of 17 kinds of phthalates in edible oil by gas chromatography-mass spectrometry. Methods The samples were extracted with acetonitrile and centrifuged at 4000 r / min for 5 min after the internal standard was added. The acetonitrile phase was purified by SILICA / PSA mixed glass column and subjected to HP-5MS column temperature-programmed separation. The samples were separated by gas chromatography-mass spectrometry Detection, selection of ion mode determination, internal standard method. Results The method showed the lowest detectable concentration was 0.1 mg / kg ~ 0.5 mg / kg, the linear range was 0.2 μg / ml ~ 2 μg / ml, r2 was 0.992 ~ 1.000, The dicarboxylic acid esters were added at the same time. The recoveries were determined. The recoveries ranged from 75.5% to 118.8% with relative standard deviations from 3.7% to 13.9%. Conclusion The method has high sensitivity, good purification effect and can rapidly and accurately determine 17 kinds of phthalates in edible oil.