高效液相色谱串联质谱法测定纺织品中六溴环十二烷
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摘要
采用高效液相色谱串联质谱法研究并优化纺织品中三种六溴环十二烷(HBCD)的检测方法。纺织样品经过丙酮自动索氏提取、浓缩、甲醇定容,采用HPLC-MS/MS对三种HBCD进行检测。HPLC-MS/MS的优化条件为:流动相V(甲醇)∶V(乙腈)∶V(水)=40∶40∶20,三种HBCD的定量离子和辅助定性离子对为:m/z 640.6/80.8和m/z 640.6/78.9。待测物质量浓度为0.01～0.50 mg/L时,线性相关系数大于0.999,α-HBCD、β-HBCD和γ-HBCD的测定低限分别为0.01 mg/kg、0.02 mg/kg、0.02 mg/kg,空白样品的加标回收率在85%～105%。
Testing methods for hexabromocyclododecane in textiles by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) is studied. Textiles are extracted with acetone by soxhlet extraction. The solution is then concentrated and diluted with methanol. The optimized testing conditions for 3 hexabromocyclododecane derives are: the mobile phase isV(methanol)∶V(acetonitrile)∶V(water) of 40∶40∶20. The linear correlation coefficient is above 0.999 in concentration range of 0.01～0.50 mg/L. And the detection limit of α-HBCD、β-HBCD and γ-HBCD are 0.01 mg/kg,0.02 mg/kg and 0.02 mg/kg, respectively. The recoveries are 85%～105% in the blank sample.
Testing methods for hexabromocyclododecane in textiles by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) is studied. Textiles are extracted with acetone by soxhlet extraction. The solution is then concentrated and diluted with methanol. The optimized testing conditions for 3 hexabromocyclododecane derives are: the mobile phase isV(methanol)∶V(acetonitrile)∶V(water) of 40∶40∶20. The linear correlation coefficient is above 0.999 in concentration range of 0.01～0.50 mg/L. And the detection limit of α-HBCD、β-HBCD and γ-HBCD are 0.01 mg/kg,0.02 mg/kg and 0.02 mg/kg, respectively. The recoveries are 85%～105% in the blank sample.
引文
[1]魏青,邢耀宇,梁必超,等.纺织品中有机卤化物的氧化裂解-离子色谱测定[J].印染,2016,42(13):45-50.
[2]陈荣圻.Oeko-Tex标准100的2009年修订版解读[J].印染,2009,35(4):44-45.
[3]程鑫,孙秀梅,金衍健,等.不同类型土壤中六溴环十二烷的浓度调查及分布特征比较[J].浙江大学学报(理工版),2018,54(4):476-483.
[4]施致雄,封锦芳,李敬光,等.超高效液相色谱-电喷雾质谱法结合同位素稀释技术检测动物源性食品中的六溴环十二烷异构体[J].色谱,2008,26(1):1-5.
[5]丁友超,曹锡忠,钱凯.LC-ESI-MS法测定纺织品中HBCD含量[J].印染,2010,36(9):36-39.
[6]石亚楠,詹发强,袁和平,等.聚苯乙烯泡沫中六溴环十二烷(HBCD)释放速率测定方法[J].环境化学,2018(2):264-270.
[2]陈荣圻.Oeko-Tex标准100的2009年修订版解读[J].印染,2009,35(4):44-45.
[3]程鑫,孙秀梅,金衍健,等.不同类型土壤中六溴环十二烷的浓度调查及分布特征比较[J].浙江大学学报(理工版),2018,54(4):476-483.
[4]施致雄,封锦芳,李敬光,等.超高效液相色谱-电喷雾质谱法结合同位素稀释技术检测动物源性食品中的六溴环十二烷异构体[J].色谱,2008,26(1):1-5.
[5]丁友超,曹锡忠,钱凯.LC-ESI-MS法测定纺织品中HBCD含量[J].印染,2010,36(9):36-39.
[6]石亚楠,詹发强,袁和平,等.聚苯乙烯泡沫中六溴环十二烷(HBCD)释放速率测定方法[J].环境化学,2018(2):264-270.