气相色谱–质谱法测定紫外光固化黏合剂中(2,4,6-三甲基苯甲酰基)二苯基氧化膦

Determination of diphenyl(2,4,6-trimethylbenzoyl)-phosphine oxide in UV curing adhesive by gas chromatography–mass spectrometry

建立测定紫外光固化黏合剂中(2,4,6-三甲基苯甲酰基)二苯基氧化膦(TPO)的气相色谱–质谱检测方法。样品在甲苯中超声萃取,采用DB–5HT型分离色谱柱(15 m×0.25 mm,0.1μm),用质谱仪进行检测,以TPO的特征离子碎片和保留时间定性,色谱峰面积定量。结果表明,TPO的质量浓度在1~20 mg/L范围内与色谱峰面积线性关系良好,相关系数为0.9997,方法检出限为0.16 mg/L,定量限为0.55 mg/L。以阴性紫外光固化黏合剂样品为样品基质,平均加标回收率为90.9%~109.0%,测定结果的相对标准偏差为1.1%~1.4%(n=6)。该方法分析时间短、重复性好、灵敏度高,适用于紫外光固化黏合剂中(2,4,6-三甲基苯甲酰基)二苯基氧化膦的快速检测。

A method for determination of diphenyl(2,4,6-trimethylbenzoyl)-phosphine oxide based UV curing adhesive by gas chromatography–mass spectrometry(GC–MS)was established.The samples were extracted by ultrasonic in toluene.DB–5HT column(15 m×0.25 mm,0.1μm)was used as the separation column and detected by mass spectrometry.The characteristic ion fragments and retention time of TPO was used for qualitative analysis,and the peak area was used for quantitative calculation.The results showed that the mass concentration of TPO had a good linear relationship with the chromatographic peak area in the range of 1–20 mg/L,the correlation coefficient was 0.9997.The limit of detection was 0.16 mg/L,and the limit of quantification was 0.55 mg/L.Negative UV curing adhesive samples were used as the sample matrix,the average recoveries rate of standard addition were 90.9%–109.0%,the relative standard deviations were 1.1%–1.4%(n=6).The method can separate the target compound in a short time with good repeatability and higher sensitivity which is suitable for the rapid determination of TPO in UV curing adhesive.