气相色谱-质谱联用技术测定丁腈橡胶中壬基酚含量

Determination of nonylphenol content in acrylonitrile-butadiene rubber by combined technology of gas chromatography-mass spectrometry

以乙醇为萃取剂,在萃取平衡时间为60 min,萃取温度为60℃,辅以超声波的条件下,对丁腈橡胶中壬基酚组分进行有效分离;随后,利用石墨化炭黑固相柱对萃取液进行纯化处理;然后,采用内标定量工作曲线建立了气相色谱-质谱联用技术测定丁腈橡胶中11种壬基酚含量的方法。结果表明:以乙醇为萃取剂,连续2次的壬基酚萃取率可达96%以上;采用选择离子检测(SIM)技术,在SIM(121-135-149)检测模式下,峰形匹配完整,信噪比高;方法加标回收率大于96%,方法检出限约为1.0μg/g,相对标准偏差为5.6%;方法准确度高、重复性好。

Nonylphenols in acrylonitrile-butadiene rubber were extracted with ethanol as extractant at the extraction equilibrium time of 60 min,extraction temperature of 60℃under ultrasound assistant condition.Subsequently,the extract was purified via carbon solid phase extraction cartridges,the combined technology of gas chromatography-mass spectrometry for determining 11 types of nonylphenols in acrylonitrile-butadiene rubber was established by internal standard quantitative working curve.The results showed that the extraction rate of nonylphenols was above 96%when the sample was successively extracted twice with ethanol.With selected ion monitoring(SIM)technology,the peaks of analytes acquired in SIM(121-135-149)mode matched well with that in scan mode,and high signal-noise ratio could be obtained.The standard recovery rate and detection limit of this test method were above 96%and about 1.0μg/g respectively,the relative standard deviation was 5.6%.This method had high accuracy and good repeatability.