Study On The Migration Of Phthalates To Liquor During Production And Storage

Phthalic acid esters(PAEs)are mainly used as the material such as plastic,rubber plasticizer and softener,in order to improve the plasticity and toughness of the plastic.Plastic materials used and the migration behavior in liquor production and storage process was traced by the GB/T21928-2008 method." Determination of Phthalates in Food Packaging Materials".Control measures was drafted according the data to ensure that the amount of PAEs in liquor was the risk assessment value of National Health Commission.The results of this study provide a scientific basis to government.The main contents are as follows:(1)Luzhou-flavor,qing scent and flavor liquor are the main three types of solid-state process in Heilongjiang province.GC-MS method was used to analyzed the PAEs in the liquor,the results showed that,no plastic materials was used in the process of brewing and fermentation.In the process of production,the pipe to connect the steamer mostly are made of PVC,pipeline of filling machine generally are silicon rubber hose,PP barrel was used to cantain base liquor temporarily.PET bottles and PE bag was widely used as packaging materials.(2)Migration experiment was carried out simulate PAEs in PVC tube and silicone migration to iliquor.The results showed that when PVC tube soaked in 38% vol liquor for 5 days,0.06 mg/kg,0.10 mg/kg and 0.06 mg/kg of DIBP,DBP and DEHP was detected.0.38 mg/kg DBP was detected when PVC tube soaked in 38% vol liquor for 10 days,0.30 mg/kg beyond the request of the Ministry of Health;PVC tube soaked in 42% vol liquor for 5 days,0.06 mg/kg,0.13 mg/kg and 0.08 mg/kg of DIBP,DBP and DEHP was detected.0.46 mg/kg DBP was detected when PVC tube soaked in 42% vol liquor for 10 days,0.30 mg/kg beyond the request of the Ministry of Health;PVC tube soaked in 50% vol liquor for 5 days,0.12 mg/kg,0.22 mg/kg and 0.08 mg/kg of DIBP,DBP and DEHP was detected.0.53 mg/kg DBP was detected when PVC tube soaked in 50% vol liquor for 10 days,0.30 mg/kg beyond the request of the Ministry of Health;PVC tube soaked in 53% vol liquor for 5 days,0.11 mg/kg,0.28 mg/kg and 0.09 mg/kg of DIBP,DBP and DEHP was detected.0.65mg/kg DBP was detected when PVC tube soaked in 53% vol liquor for 10 days,2 times of the request of the ministry of health,but DEHP and DIBP content were not beyond the request of the ministry of health.And silicone tube soaked in38% vol liquor for 15 days,0.08 mg/kg and 0.07 mg/kg of DIBP and DEHP was detected.The longest socked for 30 days,0.18 mg/kg and 0.15 mg/kg of DIBP and DEHP was detected,but DEHP and DIBP content were not beyond the request of the ministry of health.And silicone tube soaked in 42% vol liquor for 10 days,0.07 mg/kg,< 0.05 mg/kg and < 0.05 mg/kg of DIBP,DBP and DEHP was detected.Socked for 30 days,0.18 mg/kg,0.15 mg/kg and 0.16 mg/kg of DIBP,DBP and DEHP was detected,but DEHP,DBP and DIBP content were not beyond the request of the ministry of health.And silicone tube soaked in 50% vol liquor for 10 days,0.08 mg/kg,< 0.05 mg/kg and 0.08 mg/kg of DIBP,DBP and DEHP was detected.Socked for 30 days,0.20 mg/kg,0.19 mg/kg and 0.22 mg/kg of DIBP,DBP and DEHP was detected,but DEHP,DBP and DIBP content were not beyond the request of the ministry of health.And silicone tube soaked in 53% vol liquor for 10 days,0.08 mg/kg,< 0.05 mg/kg and 0.08 mg/kg of DIBP,DBP and DEHP was detected.Socked for 30 days,0.21 mg/kg,0.19 mg/kg and 0.24 mg/kg of DIBP,DBP and DEHP was detected,but DEHP,DBP and DIBP content were not beyond the request of the ministry of health.The results showed that the PAEs can be detected when PVC tube was soaked in 5 days,the amount was beyond the standard amount when PVC tube was soaked for 10 days.Silicone rubber tube can be used for 30 days within the amount of limitation.but the amount of PAEs increases with the rise of alcohol concentration.(3)The experiment to simulate PAEs migration of liquor storage,the results showed that DIBP,DBP and DEHP content is less than 0.05 mg/kg when 38% vol,42% vol,50% vol and 53% vol liquor was stored in PP or 38% vol,42% liquor in PE barrel for 5 days.When 50% vol and 53% vol liquor were stored for 5 days in PE barrel,the content of DIBP,DBP and DEHP e is 0.08 mg/kg,0.10 mg/kg and 0.08 mg/kg with in the standard of Ministry of Health;When 38% 42% liquor was stored in PET barrels for 5 days,the amount of DIBP,DBP and DEHP is less than 0.05 mg/kg,but when 50% vol and 53% vol liquor was stored in PET for 5 days,0.07 mg/kg and 0.10 mg/kg of DIBP and DEHP was detected but within the standard.Results showed that the stability of PP barrels is the best,then is the PET barrels,and the PE bag has the poorest stability.The content of PAEs migrate from PE bag to 50% vol and 53% vol liquor for 5 days is 0.10 mg/kg,0.30 mg/kg which is very close to limitation.To sum up,PVC tube and silicone tube was used in the production of liquor.PAEs was detected but within the limitation when use for 5 days,but was out of limtition when used for 10 days.Silicone rubber tube can be used for 30 days within the amount of limitation.but the amount of PAEs increases with the rise of alcohol concentration.The stability of PP barrels is the best,then is the PET barrels,and the PE bag has the poorest stability.The content of PAEs migrate from PE bag to 50% vol and 53% vol liquor for 5 days is 0.10 mg/kg,0.30 mg/kg which is very close to limitation.