气相色谱-三重四极杆质谱法测定保健酒中16种邻苯二甲酸酯类物质

建立了保健酒中16种邻苯二甲酸酯类物质(PAEs)的气相色谱-三重四极杆质谱(GC-QQQ-MS)测定法。样品采用正己烷提取,使用GC-QQQ-MS测定,监测方式为选择离子监测(SIM),利用保留时间和碎片离子丰度比值判断定性结果,利用特征离子质量色谱峰峰面积-浓度标准曲线法定量,并用建立的方法分析了81批实际样品。实验结果表明:目标化合物特征离子质量色谱峰的峰面积与其质量浓度在各自的浓度范围内线性关系良好(r²≥0.9959)。在低、中、高3个浓度的添加水平下样品加标回收率除邻苯二甲酸二甲酯(DMP)为52.3%~58.7%外,其余15种化合物为88.6%~107.3%,相对标准偏差(RSD,n=6)为0.1%~6.8%。检出限为0.002~0.061 mg/L,定量限为0.005~0.202 mg/L。该方法具有灵敏、简单、准确、线性范围宽等优点,可满足保健酒中邻苯二甲酸酯类物质的检测需要。

Determination of 16 phthalate acid ester residues in health wine by gas chromatography-triple quadrupole mass spectrometry

A method for the analysis of sixteen phthalate acid ester (PAE) residues in health wine was developed using gas chromatography-triple quadrupole mass spectrometry (GC-QQQ-MS). The health wine samples were extracted with n-hexane by liquid-liquid extraction method before analysis. The samples were detected by GC-QQQ-MS with electron impact source (EI) in selected ion monitoring (SIM) mode after extraction. The separation was performed on an HP-5MS capillary column (30 m×0.25 mm×0.25 μm) with temperature programming. The retention time and the fragment ion abundance ratio were used to judge the qualitative results, and the quantitation was performed with standard curve method of the characteristic ion chromatographic peak area-concentration. Eighty-one batches of health wine samples were detected using the method. The results showed that the method had good linear relationships with correlation coefficients (r²) not less than 0.9959. The recoveries of fifteen PAEs ranged from 88.6% to 107.3% except dimethyl phthalate (DMP) which was 52.3%-58.7% in all the three spiked levels with the relative standard deviations of 0.1%-6.8%(RSD, n=6). The limits of detection were between 0.002 mg/L to 0.061 mg/L. The limits of quantification were between 0.005mg/L and 0.202 mg/L. The method is accurate, sensitive, proprietary and suitable for the simultaneous determination of the sixteen phthalate acid esters in health wine.