超高效液相色谱法测定香型中性笔墨水中10种PAEs

建立超高效液相色谱–二极管阵列检测器测定香型中性笔墨水中邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二正丙酯(DPP)、邻苯二甲酸丁基苄酯(BBP)、邻苯二甲酸二正丁酯(DBP)、邻苯二甲酸二正戊酯(DAP)、邻苯二甲酸二环己酯(DCHP)、邻苯二甲酸二正己酯(DHP)、邻苯二甲酸二(2-乙基己基)酯(DEHP)和邻苯二甲酸二正辛酯(DNOP)10种邻苯二甲酸酯(PAEs)的方法。样品采用甲醇涡旋超声提取,色谱柱为Waters ACQUITY UPLC BEH C_(18)柱(100 mm×2.1 mm,1.7μm),以乙腈–水为流动相进行梯度洗脱,用PDA检测器检测,10 min内完成10种邻苯二甲酸酯的检测。10种邻苯二甲酸酯的质量浓度在5.0~200.0 mg/L范围内与其色谱峰面积呈良好的线性关系,线性相关系数均大于0.999,检出限为3.2~4.0 mg/kg;在高低两个添加水平下,10种邻苯二甲酸酯的回收率为96.3%~104.1%,测定结果相对标准偏差为0.1%~2.9%(n=6)。该方法样品处理简单,提取效率高,分离效果好,且灵敏度高,能快速准确测定香型中性笔墨水中10种邻苯二甲酸酯。

Determination of 10 Phthalate Esters in Fragrant Gel Ink of Roller Ball Pen by UPLC

A method of ultra-performance liquid chromatography with PDA detector (UPLC-PDA) was established for determination of the 10 phthalate estersdimethyl phthalate, diethyl phthalate, dipropyl phthalate, benzyl butyl phthalate, dibutyl phthalate, dipentyl phthalate, dicyclohexyl phthalate, dihexyl phthalate, bis(2-ethylhexyl)phthalate and di-n-octyl phthalate] in fragrant gel ink of roller ball pen. The sample was extracted by methanol using shaker and ultrasonic bath. The 10 PAEs were separated within 10 min on the Waters ACQUITY UPLC BEH C18 column(100 mm×2.1 mm, 1.7 μm) by gradient elution using acetonitrile-water as the mobile phase, and detected by PDA detector. In the range of 5-200 mg/L, the content of 10 PAEs and chromatographic peak area showed good linearity with the linear correlation of more than 0.999, and the detection limits(S/N=3) of 10 PAEs were 3.2-4.0 mg/kg. The average recoveries at high and low spiked levels were 96.3％-104.1％, and the relative standard deviations of determination results were 0.1％-2.9％(n=6). The pretreatment is simple with the high extraction efficiency, and the separation is quick and effective. The method is suitable for rapid determination of the 10 phthalate esters in fragrant gel ink of roller ball pen with high sensitivity and accuracy.