Wang Chengyun, Li Lixia, Xie Tangtang, Zhang Weiya, Liu Caiming, Zhu Naiqing
Shenzhen Entry-Exit Inspection and Quarantine Bureau, Shenzhen 518045, China.
Se Pu. 2011 Aug;29(8):731-6.
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.
建立了一种气相色谱-串联质谱（GC-MS/MS）结合微波辅助萃取（MAE）同时测定纺织品中六种禁用有机磷阻燃剂的有效方法。通过考察12种不同萃取溶剂对目标分析物的萃取效率，确定最佳条件为：以丙酮为溶剂，在76℃下微波辅助萃取30 min。然后采用GC-MS/MS在多反应监测（MRM）模式下对萃取液进行分析，各分析物浓度采用外标法进行校准。三（1-氮杂环丙基）氧化膦（TEPA）、三（2-氯乙基）磷酸酯（TCEP）、三（1,3-二氯丙基）磷酸酯（TDCP）、双（2,3-二溴丙基）磷酸酯（DDBPP）、磷酸三邻甲苯酯（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和40.48～809.60 μg/L，相关系数均不小于0.997 5，定量限（LOQ）（S/N = 10）分别为3.0、0.2、0.3、25.0、2.5和29.0 μg/kg。加标回收率为82.62%～96.88%，相对标准偏差为3.80%～8.79%。该方法成功应用于8种市售纺织品中有机磷阻燃剂的测定。实验结果表明，所建立的方法简便、快速、灵敏、准确，能够满足纺织品中禁用有机磷阻燃剂分析的要求。
