| For the inability to unify the determination of VOCs in cigarette packaging ink,which classified by printing process,a general method suitable for overall cigarette packaging ink has been established by means of HS-GC/MS.The method starts from the view of printing.The content of residual VOCs in the prints is determined by analog printing,which can intuitively reflect the harm of the ink prints on human health.The pretreatment operation is convenient and reliable,avoiding random errors caused by manual sample preparation.Combined with the mass spectrometer,the traditional chromatographic measurement technology has been improved.The method is suitable for routine detection analysis in the laboratory through evaluation and verification.The main research contents of this paper are as follows:(1)Standardized sample preparation has been realized by improving the method of sample preparation.According to the analysis requirement of matrixation treatment,the suitable matrix corrector has been selected.(2)According to the boiling ranges of VOCs,the effects of parameters of headspace injection and chromatography separation on retention time,peak shape,separation degree and detector sensitivity were investigated.When the equilibrium temperature is 80℃and the equilibrium time is 45 min,the VOCs are basically balanced between the gas phase and the liquid phase,and their response values are optimal.The VOC dedicated capillary column is used as the analytical column.The initial temperature is 40℃,and keeps for 2 min,then rises at a rate of 4℃/min to200℃,and keeps for 10 min.The split ratio is 20:1.Helium is used as the carrier gas,whose flow rate is 2.0 mL/min.When the above chromatographic conditions are satisfied,the baseline of peaks is completely separated,the shape of peaks is good,and the result of separation is satisfactory.(3)Combined with the relevant standards of the tobacco industry,this paper summarizes VOC components in cigarette packaging ink.Multiple confirmations were performed by mass spectrometry.Data of retention time,which obtained under determinate conditions,are used as a reference for the qualitative analysis.(4)Under the two quantitative methods of external standard method and internal standard method,the linear ranges,detection limits,recoveries and repeatability were investigated to evaluate and verify the determination method.The ranges of linear correlation coefficients are 0.9938~0.9998 and 0.9934~0.9998,both of which are bigger than 0.99,indicating that each VOC component has a good linear relationship within their respective content ranges.The ranges of detection limits are 0.001~0.310mg/m~2 and 0.024~0.062 mg/m~2,and the ranges of quantification limits are 0.003~0.920mg/m~2 and 0.080~0.207 mg/m~2,indicating that the method has lower detection limits.Under different spiked levels,the ranges of recoveries are 80.4%~112.2%and75.5%~113.6%,both of which are bigger than 60%,and the ranges of relative standard deviation are 0.61%~5.65%and 1.03%~3.61%,both of which are less than 6%,indicating that the method has good accuracy and precision.The ranges of repeatability are 0.26%~3.57%and 1.42%~4.85%,both of which are less than 6%,indicating that repeatability of the method meets the testing requirements. |