CAJ | 학술논문

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。
건립료보건주중16충린분이갑산지류물질（PAEs）적기상색보-삼중사겁간질보（ GC-QQQ-MS）측정법。양품채용정기완제취，사용 GC-QQQ-MS 측정，감측방식위선택리자감측（ SIM），이용보류시간화쇄편리자봉도비치판단정성결과，이용특정리자질량색보봉봉면적-농도표준곡선법정량，병용건립적방법분석료81비실제양품。실험결과표명：목표화합물특정리자질량색보봉적봉면적여기질량농도재각자적농도범위내선성관계량호（ r2≥0.9959）。재저、중、고3개농도적첨가수평하양품가표회수솔제린분이갑산이갑지（ DMP）위52.3％~58.7％외，기여15충화합물위88.6％~107.3％，상대표준편차（ RSD，n =6）위0.1％~6.8％。검출한위0.002~0.061 mg / L，정량한위0.005~0.202 mg / L。해방법구유령민、간단、준학、선성범위관등우점，가만족보건주중린분이갑산지류물질적검측수요。
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 chrom-atographic 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 corre-lation coefficients(r2 )not less than 0. 995 9. 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. 005 mg / L and 0. 202 mg / L. The method is accurate,sensitive,proprietary and suitable for the sim-ultaneous determination of the sixteen phthalate acid esters in health wine.