毛细管柱气相色谱法测定小麦粉中过氧化苯甲酰
Capillary Column GC Determination of Benzoyl Peroxide in Wheat Flour
摘 要
合成了对甲苯磺酸三正丁铵,并以二氯甲烷为溶剂,用静态法涂敷于石英毛细管色谱柱上(30 m×0.53 mm i.d.,液膜厚度为1.2 μm)作为气相色谱的固定相,对柱性能进行了考察.试验表明:此色谱固定相极性较强,对于小麦粉中过氧化苯甲酰有独特的分离作用,在3个不同的浓度水平上作方法的精密度试验,得到的相对标准偏差值在1.1%~5.0%之间,线性范围为10~100 mg·L-1(r=0.994),检出限为2.0 mg·kg-1;方法的回收率为90.5% ~95.0%.
对甲苯磺酸三正丁铵
过氧化苯甲酰
小麦粉
Gas chromatography with capillary column
Tri-n-butylammonium-p-toluenesulfonate
Benzoyl peroxide
Wheat flour
Abstract
Tri-n-butylammonium-p-toluenesulfonate was prepared and its solution in dichloromethane was applied statically to silica capillary column (i.d.0.53 mm×30 m) with 1.2 μm in liquid membrane thickness,which was used as stationary phase in gas chromatography.As shown by the results of performance test,relatively strong polarity and specific capability for separation of benzoyl peroxide from wheat flour were manifested by this stationary phase.In its application to the GC-determination of benzoyl peroxide in wheat flour,precision was tested on 3 different concentration levels,giving values of RSD′s (n=5) in the range of 1.1%-5.0%.Linear relationship between the peak area and concentration of benzoic acid was found in the range of 10 to 100 mg·L-1 (r=0.994),with a detection limit of 2.0 mg·kg-1.Recovery test was made and the results obtained were in the range of 94.3%-96.6%.
中图分类号 O657.7
所属栏目 工作简报
基金项目 辽宁省教育厅科学研究计划资助项目(2021401159)
收稿日期 2006/12/14
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备注李新华(1962-),男,辽宁营口人,教授,硕士,主要研究方向为色谱催化.
引用该论文: LI Xin-hua,ZHAO Min,KOU Deng-min,ZHANG Jing,ZHANG Yuan-yuan,ZHANG Li-li. Capillary Column GC Determination of Benzoyl Peroxide in Wheat Flour[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2007, 43(8): 655～657
李新华,赵岷,寇登民,张静,张媛媛,张黎黎. 毛细管柱气相色谱法测定小麦粉中过氧化苯甲酰[J]. 理化检验－化学分册, 2007, 43(8): 655～657
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参考文献
【1】GB/T 18415-2001小麦粉中过氧化苯甲酰的测定方法[S]．
【2】任清,黄建立.小麦粉中过氧化苯甲酰与苯甲酸总量的毛细管气相色谱法测定[J].分析化学,2004,32(2):221-224．
【3】Kong R C,Lee M L.Static coating of capillary columns using mixed solvents[J].Chromatographia,1983,17(8):451-453．
【4】Xu Bingjiu,Hu Shuguang.A simple technique for marking all-glass manifolds for capillary gas chromatography[J].Journal of High Resolution Chromatography,1992,15(11):775-778．(上接第654页)赵锦瑞,何应津,钱得根,等.8-羟基喹啉-5-磺酸-CTMAB荧光光度法测定[J].分析化学,1994,22(10):1057-1060．
【5】吴惠明,郭慧清,陈永亨,等.活性炭吸附分离-分光光度法测定硫化矿和土壤中的痕量铊[J].岩矿测试,2001,20(4):275-278．
【2】任清,黄建立.小麦粉中过氧化苯甲酰与苯甲酸总量的毛细管气相色谱法测定[J].分析化学,2004,32(2):221-224．
【3】Kong R C,Lee M L.Static coating of capillary columns using mixed solvents[J].Chromatographia,1983,17(8):451-453．
【4】Xu Bingjiu,Hu Shuguang.A simple technique for marking all-glass manifolds for capillary gas chromatography[J].Journal of High Resolution Chromatography,1992,15(11):775-778．(上接第654页)赵锦瑞,何应津,钱得根,等.8-羟基喹啉-5-磺酸-CTMAB荧光光度法测定[J].分析化学,1994,22(10):1057-1060．
【5】吴惠明,郭慧清,陈永亨,等.活性炭吸附分离-分光光度法测定硫化矿和土壤中的痕量铊[J].岩矿测试,2001,20(4):275-278．
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