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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。
Using rice flour as raw material, spiked samples containing halogenated plasticizer and ultrasonic extraction with ethyl acetate as solvent, the effects of solid-liquid ratio, ultrasonic power and ultrasonic time on extraction rate of halogenated plasticizer were discussed. The optimum conditions for extracting halogen-containing plasticizer were determined by response surface methodology, and the simultaneous determination of nine kinds of halogen-containing plasticizers in rice flour products by GC-MS was established. The nine halogen-containing plasticizers were chlorinated Paraffin-52 (CP-52), 5-chloro-2-methyl-4-isothiazolin-3-one (CMI), 1,1,2,3,3,3-hexafluoro-1- (HFP), chlorinated paraffin-42 (CP-42), chlorinated anhydride (CA), difluorochloromethane (R-22), 2- Yl) -5-chlorobenzotriazole (UV-326), quaternium-15, methyl pentachloro stearate (MPCS). The results showed that the optimum conditions for the extraction of halogenated plasticizer were: solid - liquid ratio 1:13 (m / V), ultrasonic time 20 min, ultrasonic power 120 W Under these conditions, the standard deviation of retention time of nine halogenated plasticizers was ≤0.007 and the standard deviation of peak area was ≤0.061. The detection limit was 0.01μg / kg ~ 15 mg / kg (m / m) The average recovery rate of standard samples was between 87.54 and 97.65%, with the relative standard deviation of 4.63 ~ 7.81%. The method can meet the detection requirements of the nine halogen-containing plasticizers in the rice noodles product.