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    固相萃取-毛细管区带电泳法同时测定豆制品中4种碱性染料

    Simultaneous Determination of Four Basic Dyes in Soybean Products by Capillary Zone Electrophoresis Combined with Solid Phase Extraction

    • 摘要: 采用固相萃取结合毛细管区带电泳法同时测定豆制品中碱性橙2、碱性橙21、碱性橙22和碱性嫩黄O。2.00 0 g样品经50 mmol·L-1乙酸铵溶液5.00 mL超声提取两次,提取液经Oasis HLB固相萃取柱净化,用氨水-乙腈(5+95)溶液进行洗脱,洗脱液经氮气吹干,残渣用乙腈-水(25+75)溶液溶解并定容至1.00 mL后进行毛细管区带电泳分离,分离电压为20 kV,分离温度为30℃,运行缓冲溶液为含20%(体积分数)乙腈的40 mmol·L-1磷酸二氢钾溶液(pH 2.5),采用紫外检测器,检测波长为210 nm。4种碱性染料在7 min内达到基线分离,线性范围均为1.25~50 mg·L-1,检出限(3S/N)在0.5~0.7 mg·kg-1之间。加标回收率在73.6%~93.1%之间,测定值的相对标准偏差(n=6)小于10%。

       

      Abstract: A method of capillary zone electrophoresis couple with solid phase extraction was applied to the simultaneous determination of basic orange 2, basic orange 21, basic orange 22 and auramine O in soybean products. The sample (2.000 g) was ultrasonically extracted twice with 5.00 mL of 50 mmol·L-1 ammonium acetate solution, the extract was purified on Oasis HLB solid phase extraction column and the 4 target dyes were eluted with ammonia-acetonitrile (5+95) solution. The eluent was dried-up by nitrogen blowing and the residue was dissolved and diluted to 1.00 mL with acetonitrile-H2O (25+75) solution. The target dyes were separated by capillary zone electrophoresis at 30℃ and 20 kV with 40 mmol·L-1 potassium dihydrogen phosphate solution containing 20% (φ) acetonitrile as running buffer solution (pH 2.5) and detected with a UV detector at the wavelength of 210 nm. Separation of the 4 dyes from baseline was achieved within 7 min. The linearity ranges of the four basic dyes were all 1.25-50 mg·L-1 and detection limits (3S/N) were in the range of 0.5-0.7 mg·kg-1. Recovery rates obtained by standard addition method were 73.6%-93.1%, and RSDs (n=6) were less than 10%.

       

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