摘要
以米面制品为原料,加标制成含卤增塑剂的试样,以乙酸乙酯为溶剂超声提取,探讨了固液比、超声功率和超声时间对含卤增塑剂提取率的影响,并通过响应曲面法确定提取含卤增塑剂最优条件,建立了同时对米面制品中9种含卤增塑剂进行超声提取GC-MS检测的方法,9种含卤增塑剂为氯化石蜡-52(CP-52)、5-氯-2-甲基-4-异噻唑啉-3-酮(CMI)、1,1,2,3,3,3-六氟-1-丙烯(HFP)、氯化石蜡-42(CP-42)、氯桥酸酐(CA)、二氟一氯甲烷(R-22)、2-(2-羟基-3-特丁基-5-甲基苯基)-5-氯苯并三唑(UV-326)、季铵盐-15、五氯硬脂酸甲酯(MPCS)。结果表明,提取含卤增塑剂的优选条件为:固液比1:13(m/V),超声时间20 min,超声功率120 W。在此条件下,GC-MS测定9种含卤增塑剂保留时间标准差≤0.007,峰面积标准差≤0.061,检出限为0.01μg/kg^15 mg/kg(m/m),加标试样平均回收率在87.54~97.65%之间,相对标准偏差为4.63~7.81%。该方法能满足米面制品中该9种含卤增塑剂的检测要求。
Nine kinds of halogen-containing plasticizers including chlorendic anhydride （CA）, 1,1,2,3,3,3-hexafluoro-l-Propene （HFP）, （R-22）, 5-Chloro-2-Methyl- 4-Isothiazolin -3-One （CMI）, chlorinated paraffin 42 （CP-42）, chlorinated paraffin 52 （CP-52）, 1-（3-Chloroallyl）-3,5,7-triaza-l-azoniaadamantane chloride （Quaternium-15）, 2 - （2 - hydroxy - 3 - tert-butyl -5 - methyl-phenyl） -5- （UV-326）, and pentachlorophenol methyl stearate （MPCS） were extracted by ultrasonic with ethyl acetate as solvent.. Rice and flour products were made from spiked samples as halogen-containing plasticizer. The effects of solid-liquid ratio, ultrasonic power and ultrasonic extraction time on halogen-containing plasticizers extraction yield were investigated. The optimum condition of extraction was obtained by response surface methodology test. The optimal process conditions were solid-liquid ratio of 1：13 （m/V）, extraction time of 20 min and ultrasonic power of 120 W. Under these conditions, the standard deviations of retention time and peak area were no more than 0.007 and 0.061 respectively. Detection limit of the nine kinds of halogen-containing plasticizers varied between 0.01μg/L-15 mg/L, the average recovery were between 87.54-97.65%, and the relative standard deviations were 4.63-7.81%.Therefore, the method was suitable for the extraction of the nine plasticizers mentioned above in rice and flour products.
出处
《现代食品科技》
EI
CAS
北大核心
2014年第3期250-254,共5页
Modern Food Science and Technology
基金
广东省促进科技服务业发展计划项目(2011B040300018)
关键词
含卤素类增塑剂
超声辅助提取
GC
MS
同时检测
Halogen-containing plasticizers
sonication-assisted extraction
GC-MS
simultaneous determination
