纺织学报 ›› 2014, Vol. 35 ›› Issue (7): 94-0.

• 染整与化学品 • 上一篇    下一篇

涤纶中致癌芳香胺的加速溶剂萃取-UPLC-MS/MS快速测定

吴刚1 王力君2 张明誉2 郭方龙2 赵珊红1   

    1. 浙江省检验检疫科学技术研究院
    2. 浙江立德产品技术有限公司
  • 收稿日期:2013-07-10 修回日期:2014-03-14 出版日期:2014-07-15 发布日期:2014-07-15
  • 通讯作者: 吴刚 E-mail:wg@ziq.gov.cn
  • 基金资助:

    国家质检总局科研项目;浙江省科技厅公益性资助项目

Determination of aromatic amines in terylene by ASE coupled with UPLC-MS/MS

  • Received:2013-07-10 Revised:2014-03-14 Online:2014-07-15 Published:2014-07-15
  • Contact: WU Gang E-mail:wg@ziq.gov.cn

摘要: 利用加速溶剂萃取结合超高效液相色谱-串联质谱(UPLC-MS∕MS)技术,建立了一种能在6min内快速分离和测定涤纶中禁用偶氮染色剂可分解出的22种致癌芳香胺的方法。样品经丙酮加速溶剂萃取、浓缩,再经氧化-还原裂解反应,用乙酸乙酯萃取反应液中的芳香胺,再将萃取液用N2吹至近干,用甲醇-水溶液(1∶9,v∶v)溶解定容,采用Acquity UPLC BEH C18柱(100 mm × 2.1 mm,1.7 μm)分离,以甲醇-0.05%甲酸溶液为流动相,梯度洗脱,电喷雾正离子模式多反应监测,外标法定量。该方法在0.01~0.2 μg/mL范围内线性关系良好(γ>0.99),在添加浓度为15 ~ 30 mg/kg水平内,平均回收率范围为33.28 ± 1.83~ 107.14 ± 1.10 %,相对标准偏差(RSD)为0.38 ~ 10.9%,方法检出限(LOD)为0.96 ~ 17 μg/kg,方法定量限(LOQ)为3.2 ~ 56.1 μg/kg。本方法样品前处理自动化程度高,操作过程简便快速,重复性好,能满足涤纶中的可分解出致癌芳香胺的禁用偶氮染色剂的快速筛选与测定。

关键词: 加速溶剂萃取, 超高效液相色谱-串联质谱, 涤纶, 禁用偶氮染料

Abstract: A novel method has been developed for the rapid extraction and determination of 22 aromatic amines derived from banned azo colorants in terylene by accelerated solvent extraction (ASE) with acetone coupled with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The extract was dried by rotavapor, then through REDOX cracking reaction, and then using ethyl acetate to extract aromatic amines from the reaction liquid. The extract was blowed with N2 to nearly dry, redissolved in the solvent of methanol and water(1∶9,v∶v).The chromatographic analysis was performed on an acquity UPLC BEH C18 column (100 mm × 2.1 mm,1.7 μm ) by a gradient elution employing of methanol and 0.05% formic acid as a mobile phase. The analytes were detected by electrospray ionization (ESI) tandem mass spectrometry with multiple reaction monitoring (MRM) in positive ion mode. Good linearity (r > 0.99) was observed between 0.01 and 0.2 μg/mL for all compounds. The recoveries and relative standard deviations (RSDs) were checked by spiking untreated samples with the 22 aromatic amines at three levels: 15, 20 and 30 mg /kg. The average recoveries of the 22 aromatic amines were from 33.28 ± 1.83 to 107.14 ± 1.10%. The precision values expressed as RSD were from 0.38 to 10.9% (n = 6). The limits of detection were from 0.96 to 17 μg/kg, and the limits of quantification were 3.2 to 56.1 μg/kg for the analytes. The results showed that the method can be considered a fast and easy alternative technique with great ruggedness, high degree of automation and good suitability for screening and detecting 22 aromatic amines derived from banned azo colorants in terylene.

Key words: ASE, UPLC-MS∕MS, terylene, banned azo dye

[1] 王嘉欣 田秀枝 蒋学 王鸿博 高卫东. 二醛 β-环糊精/壳聚糖改性对涤纶织物亲水性能的影响[J]. 纺织学报, 2018, 39(07): 82-88.
[2] 秦传香 鲍志敏 戴礼兴 梅锋. 新型萘酰亚胺类荧光染料的合成及其染色应用[J]. 纺织学报, 2018, 39(07): 74-81.
[3] 蓝舟 瞿建刚 王春梅 徐俊芳 钱佳琪. 纤维基钒酸铋的制备及其光催化性能[J]. 纺织学报, 2018, 39(06): 89-95.
[4] 陈永邦 黄成 阎克路 叶敬平. 导湿排汗涤纶针织物的抗菌亲水整理[J]. 纺织学报, 2018, 39(05): 74-79.
[5] 李敏 赵影 张丽平 张奕 付少海. 涤纶针织物数码印花清晰度的影响因素[J]. 纺织学报, 2018, 39(05): 62-66.
[6] 葛陈程 吕汪洋 石教学 徐铁凤 陈世昌 李楠 陈文兴. 应用二维X射线衍射法测定涤纶工业丝结晶和取向行为[J]. 纺织学报, 2018, 39(03): 19-25.
[7] 刘凡 钱晓明 赵宝宝 钱幺 朵永超. 柔软处理对涤纶/锦纶6中空桔瓣型超细纤维非织造布性能的影响[J]. 纺织学报, 2018, 39(03): 114-119.
[8] 郑君红 李亮 刘让同 张丹. 羊毛角蛋白的制备及其对涤纶织物的整理[J]. 纺织学报, 2018, 39(03): 92-97.
[9] 卢声 林杰 路艳华 黄凤远 程德红. 用含三嗪结构苯基磷酸酯的涤纶织物阻燃整理[J]. 纺织学报, 2018, 39(03): 98-102.
[10] 韩潇 洪剑寒 惠林 史韩萍 金丽华. 导电涤纶纱连续制备工艺与性能[J]. 纺织学报, 2018, 39(02): 20-25.
[11] 黄婕妤 吕鹏飞 姚壹鑫 魏取福. 细菌纤维素/涤纶非织造布自编织复合材料的制备及其性能[J]. 纺织学报, 2018, 39(02): 126-131.
[12] 陈莹 王鸿达 李宥宣. 不同溶剂对聚吡咯/涤纶材料抗凝血性能的影响[J]. 纺织学报, 2018, 39(02): 132-137.
[13] 叶思佳 杜奕铃 张永高 郑今欢. 涤纶起绒织物着色烂花印花中分散染料的耐碱性[J]. 纺织学报, 2018, 39(01): 98-103.
[14] 曹机良 孟春丽 曹毅 闫凯 吴宁杰 王潮霞. 烷基咪唑类双子型离子液体对涤纶织物的碱减量处理[J]. 纺织学报, 2018, 39(01): 79-83.
[15] 李静 王晓 邵伟 崔永珠 魏春艳. 改性活性染料对涤纶织物的紫外光引发接枝染色[J]. 纺织学报, 2017, 38(11): 91-96.
Viewed
Full text


Abstract

Cited

  Shared   
  Discussed   
No Suggested Reading articles found!