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建立了超高效液相色谱-静电场轨道阱高分辨质谱(UPLC/OrbitrapHRMS)同时测定涂布纸中多种邻苯二甲酸酯类增塑剂的方法,该方法以三氯甲烷为萃取溶剂,超声萃取涂布纸中的邻苯二甲酸酯类增塑剂,提取液经处理后进行UPLC/OrbitrapHRMS分析,外标法定量。样品用Hypersil GOLD色谱柱(100mm×2.1mm×1.9μm)进行分离,以5mmol/L乙酸铵水溶液(含0.1%甲酸)/甲醇为流动相,电喷雾正离子(ESI+)模式进行电离,以保留时间和准分子峰的精确质量数定性,以提取色谱峰的面积定量。23种邻苯二甲酸酯类增塑剂的质量准确度小于3mg/kg,在各自线性范围内,各组分线性良好,线性相关系数均大于0.997,检出限为0.1μg/kg~2.0μg/kg。在3个不同浓度的加标水平下,方法的加标平均回收率为80.2%~93.1%,相对标准偏差(RSD,n=9)为3.3%~9.9%。该方法定性可靠,定量准确,灵敏度高。采用该方法对市售涂布纸进行测定,在部分样品中检出不同含量水平的多种邻苯二甲酸酯类增塑剂。
A method for the simultaneous determination of various phthalate plasticizers in coated paper by UPLC / OrbitrapHRMS was established. The method uses chloroform as the extraction solvent, Ultrasound extraction of phthalate plasticizer coated paper, the extract was processed after UPLC / OrbitrapHRMS analysis, external standard. The sample was separated on a Hypersil GOLD column (100 mm × 2.1 mm × 1.9 μm) and ionized in a 5 mmol / L ammonium acetate aqueous solution (containing 0.1% formic acid) in methanol as the electrospray positive ion (ESI +) mode to retain The exact masses of time and excimer peaks are quantified to extract the area of the chromatographic peaks. The mass accuracy of 23 kinds of phthalate plasticizers was less than 3mg / kg. The linearity of each component was linear with linear correlation coefficient greater than 0.997 and the detection limit was 0.1μg / kg ~ 2.0μg / kg. The average recoveries of spiked samples were 80.2% -93.1% at 3 spiked levels, with relative standard deviations (RSDs, n = 9) of 3.3% -9.9%. The method is qualitative and reliable, quantitative and accurate, high sensitivity. The method was applied to the determination of commercially available coated paper, and various phthalate plasticizers with different content levels were detected in some samples.