Determination Of The PFCs In Textiles By In-Capillary SPE-GC/MS Coupled With Derivatization

PFCs as a kind of surface active agent,is widely used in textile,leather and other industries,they can enter biological body through food,breathing and other way,cause a harm to human.Therefore,it is necessary to detect PFCs in textiles.Traditional GC/MS detection of PFCs derivative reaction,and the common derivative reaction is conducted before extraction into salt,and then by GC/MS to detect the derivative of this compound.In this paper,a salt reactive –in-capillary SPE-GC/MS method was developed to detect PFCs technology,which solves the problem of complicated intermediate process and low sample utilization.The research contents are as follows:(1)The efficiency of the salt reaction will affect the subsequent detection effect,so it is necessary to discuss the salt condition.This experiment based on different ultrasonic temperature,ultrasonic time and ultrasonic power comparison,get when the ultrasonic temperature reaches 45 ?,the ultrasonic power is 80 W,ultrasonic time is 40 min as salt effect is best.(2)Three different solid-phase extraction columns were selected: C18 column,Oasis MAX column,and Oasis WAX column,and a selection of PFCs extraction effect of best the types of the solid phase extraction solven,the amount of the elution agent,the elution rate were optimized.The results showed that the optimal solid phase extraction column was Oasis WAX column,5 mL with methanol and water(80:20,V/V)as eluent,the elution rate of 3 mL/min.(3)A method for detecting PFCs in textiles by In-Capillary SPE-GC/MS coupled with derivatization was established.Using Oasis WAX column as filling agent in capillary-SPE column,determine the best extraction conditions of in capillary-SPE column,1.2?L ultrapure water and methanol activation,1.2?L with methanol and water(80:20,V/V)as eluent loading velocity is 0.5 ?L/min,hot stripping,to within the capillary length is 4.5 cm SPE column as a manual injector direct manual sampling,sample time retention is 3s.Through the verification of this method,it is found that this method has more than 100 times the enrichment multiple of PFCs.The linear correlation coefficients of two PFCs were greater than 0.998,and the linear correlation was good.The standard deviation was less than 4.0% between 89.24% and 103.21%.It is proved that this method is feasible.