Determination Of Plasticizer In Textiles By UPLC-MS/MS

Nineteen kinds of plasticizer,including DMP,DEP,DPROP,DIBP,DBP,DPP,DHP,DCHP,DEHP,DNOP,DINP,DIDP,DMEP,DEEP,DBEP,DPHP,BBP,DAP and DINCH were selected as object in this dissertation.Through continuous exploration experiment,a quick confirming method was developed in this dissertation to determine 19 kinds of plasticizer in textiles by ulta performance liquid chromatography-tandem quadrupole mass spectrometry(UPLC-MS/MS),and the method is used for the detection of real samples.The main results were got as following:(1)Through the UPLC-MS/MS mass spectrometry and chromatographic conditions were optimized,19 kinds of plasticizer were completely separated.The optimal conditions for UPLC-MS/MS were obtained as follows: ACQUITY UPLC C18 column(100mm×2.1mm,1.7?m)with a mobile phase methanol-water in gradient elution mode at the flow rate of 0.4 ?L/min,in which the water phase was added 0.1%formic acid;oven temperature was 50?;injection volume of liquid sample was 2?L;electrospray ionization;Source temperature was 150?;Monitoring mode: multiple reaction monitoring(MRM).(2)Through the selection experiment of main influencing factors of microwave assisted extraction,the optimal experimental conditions were determined as follows:acetonitrile extraction solvent,the temperature was 101?,the extraction time was 30 min.In the range of 0.1 ~ 5?g/m L,the linearity of method was good and the correlation coefficients were over 0.994;The LOQ of the method with in 0.2 ~1mg/kg,the LOD of the method with in 0.1~0.2mg/kg.After microwave assisted extraction,printing,coating and PU fabric were added a series of standard solutions,the average recovery were 88.8% ~ 88.8%,89.2% ~ 111.9%,and 89.6% ~ 113.5%,precision(n = 6)were 0.8% ~ 0.8%,1.0% ~ 10.9%,and 1.3% ~ 12.1%.(3)Four factors three levels orthogonal experiment was established by extraction solvent,temperature,time and power,which were the main effect factor of ultrasonic assisted extraction.The optimal experimental conditions were determined as follows:extraction solvent was methylene chloride,the extraction time was 40 min,the temperature was 30 ?,the power was 100%.In the range of 0.1 ~ 5?g/m L,the linearity of method was good and the correlation coefficients were over 0.994;The LOQ of the method with in 0.1~1.5mg/kg,the LOD of the method was 0.1mg/kg.After ultrasonic assisted extraction,printing,coating and PU fabric were added a series of standard solutions,the average recovery were86.6%~112.9%,86.6%~113.9%,and 84.9%~113.5%,precision(n = 6)were 1.1%~10.1%,1.4%~10.1%,and 1.1%~9.9%.(4)The main component of the synthetic uncertainty includes sample quality,standard stock solution preparation,the middle of standard stock solution preparation,standard work,standard curve fitting,recovery,repeatability.The larger contribution to the synthesis of uncertainty are standard curve fitting?recovery?repeatability,the middle of standard stock solution preparation and standard work in the middle of the contribution,the contribution of standard stock solution is small,and contribution to the minimum sample weighing,which can be neglected.This article contains 19 figures,50 tables and 74 references.