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

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。

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

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 degrees C 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 microg/L, respectively, the correlation coefficients were not less than 0.997 5, while the limits of quantification (LOQ) (S/N = 10) were 3.0, 0.2, 0.3, 25.0, 2.5 and 29.0 microg/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.