离子迁移谱快速筛查白酒中痕量邻苯二甲酸酯的研究
建立了离子迁移谱技术快速检测白酒中痕量邻苯二甲酸酯的方法。对迁移管温度、进样口温度进行了参数优化后,选取5种典型的邻苯二甲酸酯进行了系统研究。在迁移管和进样口温度分别为90℃和160℃的条件下,邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯、邻苯二甲酸二异丁酯和邻苯二甲酸二（2-乙基己）酯的检出限分别为0.14,0.06,0.14,0.44和0.02 mg/L;9次平行测量的相对标准偏差RSD〈8.9%,单个样品的分析周期小于95 s。将本方法应用于5种白酒盲样的检测,成功筛查出邻苯二甲酸酯类物质。利用离子阱质谱对5种邻苯二甲酸酯标样产物离子和白酒盲样的产物离子进行了确认,结果表明,离子...
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| Published in | 分析化学 Vol. 42; no. 2; pp. 278 - 282 |
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| Main Author | |
| Format | Journal Article |
| Language | Chinese |
| Published |
中国科学院研究生院,北京100039%中国科学院大连化学物理研究所,大连,116023
2014
中国科学院大连化学物理研究所,大连116023 |
| Subjects | |
| Online Access | Get full text |
| ISSN | 0253-3820 |
| DOI | 10.3724/SP.J.1096.2014.30730 |
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| Summary: | 建立了离子迁移谱技术快速检测白酒中痕量邻苯二甲酸酯的方法。对迁移管温度、进样口温度进行了参数优化后,选取5种典型的邻苯二甲酸酯进行了系统研究。在迁移管和进样口温度分别为90℃和160℃的条件下,邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯、邻苯二甲酸二异丁酯和邻苯二甲酸二（2-乙基己）酯的检出限分别为0.14,0.06,0.14,0.44和0.02 mg/L;9次平行测量的相对标准偏差RSD〈8.9%,单个样品的分析周期小于95 s。将本方法应用于5种白酒盲样的检测,成功筛查出邻苯二甲酸酯类物质。利用离子阱质谱对5种邻苯二甲酸酯标样产物离子和白酒盲样的产物离子进行了确认,结果表明,离子迁移谱的谱峰是邻苯二甲酸酯离子。这说明丙酮作为掺杂剂,可以避免白酒中背景化合物的干扰。本方法适于大量白酒样品中邻苯二甲酸酯类物质的快速筛查。 |
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| Bibliography: | Phthalic acid ester is a kind of common environmental pollutants. Here, a method for fast screening trace phthalic acid ester in wine was constructed based on ion mobility spectrometry （IMS）. Tube temperature and inlet temperature were optimized, and five typical phthalic acid esters were detected successively. Under the optimal tube temperature of 90℃ and inlet temperature of 160℃, the limits of detection for dimethyl phthalate （DMP）, diethyl phthalate （ DEP）, dibutyl phthalate （ DBP）, diisobutyl phthalate （DIBP） and diethylhexyl phthalate （DEHP） are 0.14, 0.06, 0.14, 0.44 and 0.02 nag/L, respectively, and the relative standard deviation （RSD） of 9 times measurements are less than 8.9%. The analytical time for single sample is less than 95 s. At last, five types of white wines were analyzed and the suspicious problem samples were successfully screened. And a home-made ion trap mass spectrometer was used to verify the product ions of phthalic acid ester detected by IMS and the interferences in wines can be av |
| ISSN: | 0253-3820 |
| DOI: | 10.3724/SP.J.1096.2014.30730 |