色谱

色谱

• 研究论文 • 上一篇    下一篇

磁性多壁碳纳米管固相萃取-气相色谱-质谱法检测水样中的13种邻苯二甲酸酯类化合物

付善良, 丁利, 朱绍华, 焦艳娜, 龚强, 陈继涛, 吴新华, 王利兵*   

  1. 湖南省检验检疫科学研究院, 湖南出入境检验检疫局技术中心, 食品安全科学技术湖南省重点实验室, 湖南 长沙 410004
  • 收稿日期:2011-03-15 修回日期:2011-04-27 出版日期:2011-08-28 发布日期:2011-09-28
  • 通讯作者: 王利兵,博士,研究员,研究方向为食品安全与检验检疫安全

Simultaneous determination of six organophosphorous flame retardants in textiles by gas chromatography-tandem mass spectrometry combined with microwave assisted extraction

FU Shanliang, DING Li, ZHU Shaohua, JIAO Yanna, GONG Qiang, CHEN Jitao, WU Xinhua, WANG Libing*   

  1. Hunan Academy of Inspection and Quarantine, Technology Center of Hunan Entry-Exit Inspection and Quarantine Bureau, Hunan Key Laboratory of Food Safety Science & Technology, Changsha 410004, China
  • Received:2011-03-15 Revised:2011-04-27 Online:2011-08-28 Published:2011-09-28

PDF

618

被引次数

59

摘要： 建立了磁性多壁碳纳米管(MWCNTs)固相萃取结合气相色谱-质谱检测水样中13种邻苯二甲酸酯类化合物(PAEs)的方法。优化了萃取时间、水样pH值、解吸溶剂的种类和用量、解吸时间等影响萃取效率的主要条件。最终确定萃取时间为10 min,水样pH 5～7,解吸溶剂为2 mL丙酮,解吸时间为5 min。在优化的条件下,各组分的萃取回收率为89.7%～100.5%。方法具有较高的灵敏度,检出限(信噪比(S/N)为3)为0.08～0.47 μg/L。3种实际样品的加标回收率为84.5%～107.5%,相对标准偏差为1.9%～12.8%。该方法操作简便、省时,准确、灵敏、环保,可用于水样中PAEs的检测,并成功地应用于自来水、瓶装饮用水和湖水样品的分析,13种PAEs均未检出。

关键词: 磁性多壁碳纳米管, 固相萃取, 邻苯二甲酸酯类化合物, 气相色谱-质谱, 水样

Abstract: An effective method was established for the simultaneous determination of six banned organophosphorous flame retardants in textiles by gas chromatography-tandem mass spectrometry (GC-MS/MS) combined with microwave assisted extraction (MAE). By investigating the extraction efficiency of 12 different extraction solvents for the target analytes, the optimal conditions were that the sample was extracted by microwave assisted extraction using acetone as the solvent at 76 ℃ for 30 min. Then the extract was analyzed by GC-MS/MS in multiple reaction monitoring (MRM) mode, and the concentration of each analyte was calibrated by external standard method. The linear ranges of tris-(1-aziridinyl)phosphine oxide (TEPA), tris-(2-chloroethyl)phosphate (TCEP), tris-(1,3-dichloropropyl)phosphate (TDCP), bis-(2,3-dibromopropyl)phosphate (DDBPP), tri-o-cresyl phosphate (TOCP) and tris-(2,3-dibromopropyl)phosphate (TRIS) were 9.17~366.80, 0.95~75.98, 1.04~83.20, 41.60~832.00, 3.80~75.90, and 40.48~809.60 μg/L, respectively, the correlation coefficients were not less than 0.9975, while the limits of quantification (LOQ) (S/N=10) were 3.0, 0.2, 0.3, 25.0, 2.5 and 29.0 μg/kg, respectively. The spiked recoveries varied from 82.62% to 96.88% with the relative standard deviations of 3.80% to 8.79%. The proposed method was successfully applied to the determination of organophosphorous flame retardants in eight commercial textiles. The experimental results demonstrated that the method developed is simple, rapid, sensitive and accurate, which could satisfy the demand of the analysis of banned organophosphorous flame retardants in textiles.

Key words: gas chromatography-mass spectrometry （GC-MS）, phthalate acid esters, water samples, magnetic multi-walled carbon nanotubes, solid phase extraction （SPE）