摘要
建立了微乳毛细管电动色谱法分离检测12种邻苯二甲酸酯类(PAEs)增塑剂的方法。考察了缓冲液类型及质量浓度、pH、表面活性剂十二烷基硫酸钠(SDS)质量浓度、助表面活性剂质量浓度、乙腈体积分数等对12种PAEs分离的影响。结果表明,最佳的微乳液组成为:质量浓度为33.1mg/mL的SDS、66.1mg/mL的正丁醇、8.1mg/mL的正辛烷,体积分数为12%的乙腈、77.3%的6mmol/L磷酸盐-硼砂缓冲液(pH值为9.0)。当分离温度为20℃,分离电压为20kV,检测波长230nm时,12种PAEs在20min内达到基线分离。12种PAEs的平均回收率和精密度分别为85.3%~96.9%和3.4%~6.8%,方法检出限(S/N=3)低至0.5μg/mL。该方法操作简便,灵敏度较高,试验结果准确可靠,可用于黄酒样品中12种PAEs的检测,结果满意。
A microemulsion electrokinetic chromatographic(MEEKC)method was developed to separate and detect 12 phthalate acid esters(PAEs)in rice wine.A variety of factors were examined,including pH values,and mass concentration of buffer solution,sodium dodecyl sulfate(SDS)surfactant,co-surfactant,volume fraction of acetonitrile,in order to optimize their effects on the separations of 12 PAEs.The results indicated that an optimal MEEKC separation method was achieved by using a microemulsion solution of pH 9.0 containing 33.1 mg/mL(w/v)SDS,66.1 mg/mL(w/v)1-butanol,8.1 mg/mL(w/v)octane,12%(v/v)acetonitrile and 77.3%(v/v)6 mmol/L phosphateborax buffer solution.The 12 PAEs were baseline separated within 20 min at 20 kV and 20℃,when the detection wavelength being 230 nm.Under the optimized experimental conditions,the average recoveries and precision rates of 12 PAEs were in the ranges of 85.3%~96.9% and 3.4%~6.8%,respectively.The lowest limit of detection(LOD)was 0.5(μg/mL).The MEEKC method,simple in operation,high in sensitivity and reliable in result,has been successfully applied for the analysis of 12 PAEs in rice wine with satisfactory results.
作者
黄琦
季晓娟
徐立锋
HUANG Qi;JI Xiaojuan;XU Lifeng(School of Biological and Chemical Engineering,Zhejiang University of Science and Technology,Hangzhou 310023,Zhejiang,China;Zhejiang Provincial Key Laboratory for Chemical and Biological Processing Technology of Farm Produce,Hangzhou 310023,Zhejiang,China)
出处
《浙江科技学院学报》
CAS
2018年第3期187-192,共6页
Journal of Zhejiang University of Science and Technology
基金
浙江省分析测试科技计划研究项目(2015C37072)
关键词
微乳毛细管电动色谱法
邻苯二甲酸酯
黄酒
microemulsion capillary electrokinetic chromatography
phthalate acid esters
rice wine