CAJ | 학술논문

建立了纺织品中9种有机磷酸酯类阻燃剂的超高效液相色谱-串联质谱( UHPLC-MS/MS)测定方法。样品在密闭萃取瓶中于50℃用甲醇超声萃取30 min,萃取液过滤后直接进样；采用C18色谱柱分离、甲醇/水(含5.0 mmol/L甲酸铵)为流动相,进行梯度洗脱,电喷雾正离子模式电离,多重反应监测模式测定,外标法定量。实验优化了纺织样品的超声萃取条件及色谱分离、质谱测定条件,对不同类型纺织样品的基质效应进行详细研究并拟定了基质效应消除/补偿技术。优化实验条件下,方法的精密度( RSD, n=5)分别为棉布5.2％(TOCP)~12.5％(TRIS)、聚酯纤维6.4％(TBEP)~13.8％(TRIS)、羊毛6.9％(TDCP)~14.5％(TEPA)；在上述类型纺织品添加低、中、高3个浓度水平时,加标回收率在52.5％(TEPA)~116.4％(TPP)之间；方法定量限(LOQ, S/N=10)为1.0(TBP)~10.0(TRIS)μg/kg。方法具有样品前处理简单,分析速度快、选择性好的特点,适用于纺织品中多种有机磷酸酯类阻燃剂的准确测定。
건립료방직품중9충유궤린산지류조연제적초고효액상색보-천련질보( UHPLC-MS/MS)측정방법。양품재밀폐췌취병중우50℃용갑순초성췌취30 min,췌취액과려후직접진양；채용C18색보주분리、갑순/수(함5.0 mmol/L갑산안)위류동상,진행제도세탈,전분무정리자모식전리,다중반응감측모식측정,외표법정량。실험우화료방직양품적초성췌취조건급색보분리、질보측정조건,대불동류형방직양품적기질효응진행상세연구병의정료기질효응소제/보상기술。우화실험조건하,방법적정밀도( RSD, n=5)분별위면포5.2％(TOCP)~12.5％(TRIS)、취지섬유6.4％(TBEP)~13.8％(TRIS)、양모6.9％(TDCP)~14.5％(TEPA)；재상술류형방직품첨가저、중、고3개농도수평시,가표회수솔재52.5％(TEPA)~116.4％(TPP)지간；방법정량한(LOQ, S/N=10)위1.0(TBP)~10.0(TRIS)μg/kg。방법구유양품전처리간단,분석속도쾌、선택성호적특점,괄용우방직품중다충유궤린산지류조연제적준학측정。
A rapid method was developed for the determination of 9 organophosphorous flame retardants ( OPFRs) in textiles by ultra high performance liquid chromatography tandem electrospray ionization mass spectrometry ( UHPLC-MS/MS ) . Analytes in textile samples were extracted in a closed bottle at 50℃ with methanol by ultrasonic extraction for 30 min. And then, the extracted solution was injected after filtration and determined by UHPLC-MS/MS. Target analytes were separated by C18 column and methanol/water containing 5. 0 mmol/L NH4 COOH. The positive electrospray ionization and multiple reaction monitoring mode ( MRM) was utilized. The matrix effect (ME) could be compensated by adjusting the concentration of NH4COOH and the composition of the mobile phase after careful investigation with blank samples. An external standard calibration method was chosen to the quantitative analysis. Under the optimized conditions, method precision represent with relative standard deviations (RSDs) was 5. 2% (TOCP) -12. 5% (TRIS) for cotton, 6. 4%(TBEP)-13. 8% (TRIS) for polyester, and 6. 9% (TDCP) -14. 5% (TEPA) for wool samples. The recoveries for standard addition were in the range of 52 . 5% ( TEPA ) -116 . 4% ( TPP ) . The limits of quantification (LOQ, S/N=10) were between 1. 0 (TBP) and 10. 0 (TRIS) μg/kg.