微乳毛细管电动色谱法检测黄酒中邻苯二甲酸酯类增塑剂

Detection of phthalate acid esters in rice wine by microemulsion capillary electrokinetic chromatography

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.