气质联用法同时测定米面制品中9种含卤素增塑剂的研究.pdfVIP

现代食品科技 Modern Food Science and Technology 2014, Vol.30, No.3 气质联用法同时测定米面制品中的9种含卤素增塑剂 皮小弟，李叶青，曾石峭，成莲，殷兆平，俆育成 （广东省河源市质量计量监督检测所，广东河源 517000） 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0.01 μg/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。 关键词：含卤素类增塑剂；超声辅助提取；GC-MS；同时检测 文章篇号：1673-9078(2014)3-250-254 Simultaneous Determination of Nine Kinds Halogen-containing Plasticizers in Rice and Flour Products by GC–MS PI Xiao-di, LI Ye-qing, ZENG Shi-qiao, CHENG Lian, YIN Zhao-ping, XU Yu-cheng (Heyuan Supervision Testing Institute of Quality and Metrology, Guangdong, Heyuan517000, China) Abstract: Nine kinds of halogen-containing plasticizers including chlorendic anhydride (CA), 1,1,2,3,3,3-hexafluoro-1-Propene (HFP), difluoro-chloromethane (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-1-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 hal