色谱

色谱

• 研究论文 • 上一篇    下一篇

微波辅助萃取-气相色谱/串联质谱法快速测定纺织品中禁用有机磷阻燃剂

王成云*, 李丽霞, 谢堂堂, 张伟亚, 刘彩明, 褚乃清   

  1. 深圳出入境检验检疫局, 广东 深圳 518045
  • 收稿日期:2011-03-07 修回日期:2011-04-08 出版日期:2011-08-28 发布日期:2011-09-28
  • 通讯作者: 王成云,博士,高级工程师. Tel: (0755)83886224
  • 基金资助:

    深圳出入境检验检疫局科技计划项目(SZ2010014)和国家认监委科研制标项目(2011B238k)

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

WANG Chengyun*, LI Lixia, XIE Tangtang, ZHANG Weiya, LIU Caiming, ZHU Naiqing   

  1. Shenzhen Entry-Exit Inspection and Quarantine Bureau, Shenzhen 518045, China
  • Received:2011-03-07 Revised:2011-04-08 Online:2011-08-28 Published:2011-09-28

PDF

656

被引次数

11

摘要： 以丙酮为萃取溶剂，采用微波辅助萃取技术对纺织品中禁用有机磷阻燃剂进行萃取，萃取液进行气相色谱/串联质谱测定，从而建立了一种微波萃取-气相色谱/串联质谱分析方法，对纺织品中禁用有机磷阻燃剂进行了测定。6种禁用有机磷阻燃剂三-(1-氮杂环丙烯基)氧化膦(TEPA)、三-(2-氯乙基)磷酸酯(TCEP)、三-(2,3-二氯丙基)磷酸酯(TDCP)、二-(2,3-二溴丙基)磷酸酯(DDBPP)、三-(邻甲苯基)磷酸酯(TOCP)和三-(2,3-二溴丙基)磷酸酯(TRIS)的线性范围分别为9.17~366.80、0.95~75.98、1.04~83.20、41.60~832.00、3.80~75.90、40.48~809.60 ?g/L，在S/N=10的条件下，检出限分别为3.0、0.2、0.3、25.0、2.5、29.0 ?g/kg。方法精密度为3.80~8.79 %，回收率为82.62~96.88 %。气相色谱/串联质谱母离子和子离子一一对应的多反应监测模式有效地去除了基体杂质干扰和假阳性现象。该方法简便快速、灵敏度高，定性准确，可完全满足纺织品中禁用有机磷阻燃剂的检测要求。

关键词: 调味料, 防腐剂, 固相萃取;超高效液相色谱-串联质谱, 抗氧化剂

Abstract: An ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) method was developed for the simultaneous determination of 11 preservatives and 6 antioxidants in condiments. The condiment sample with low fat or middle fat was diluted with saturated NaCl solution (adjusting pH to 2~3 with phosphoric acid), then extracted with acetonitrile. The extract was purified using liquid-liquid extraction with hexane, and the sample with middle fat was further purified using solid phase extraction with a C8 column. The condiment sample with high fat was diluted with hexane, then dissolved with saturated NaCl solution (adjusting pH to 2~3 with phosphoric acid), and extracted with acetonitrile. The extract was purified using solid phase extraction with a C8 column. The analysis was performed on a C18 column (150 mm×2.1 mm, 1.7 μm) using a gradient elution with the mobile phases of 20 mmol/L ammonium acetate buffer and acetonitrile, and determined by tandem mass spectrometry in negtive ESI mode under multiple reaction monitoring (MRM) mode. The method had good linearity (r≥0.9955). The limits of quantification (LOQs) (S/N=10) of 17 analytes ranged from 0.05 mg/kg to 5 mg/kg. The recoveries ranged from 79.7% to 118% at three spiked levels, the relative standard deviations (RSDs) ranged from 0.57% to 13.1%. The method can be applied for the determination of preservatives and antioxidants in condiments.

Key words: ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）, antioxidants, condiments, preservatives, solid phase extraction (SPE)