反向高效液相色谱-荧光法测定酒精饮料中吖啶的含量

建立酒精饮料中有机染料吖啶的反向高效液相色谱定量检测方法。样品经过0.2μm孔径的有机系微孔滤膜过滤后经C18(4.6 mm×250 mm,5μm)反相色谱柱以甲醇和水(80∶20)为流动相进行等度洗脱,温度为35℃,流速为1.0 mL/min,荧光激发光波长248 nm,荧光发射波长447 nm,流通池温度45℃,外标法定量。结果表明,吖啶进样量在2 pg^2μg时,与峰面积呈现良好的线性关系(R2=0.9999),样品中吖啶的检出限为0.083μg/L,定量限为0.275μg/L,分析时间为12 min,加标浓度为1μg/L、10μg/L和100μg/L的回收率为47%~130%,相对标准差为0.5%~2.0%。该方法操作简单,无需复杂的前处理,准确度和灵敏度较高,检测投入较低,适合酒精饮料生产企业开展酒精饮品中吖啶含量的日常检测。

Determination of Acridine Content in Alcoholic Beverages by RP-HPLC-FLD

A method for the determination of acridine content in alcoholic beverages by reversed-phase high performance liquid chromatography with fluorescence detector had been developed as follows:the samples were separated on a C18 column(4.6 mm×250 mm,5μm)at 35℃using methanol and water solution(80∶20,V/V)as the mobile phase at a flow rate of 1.0 mL/min after filtered through a 0.2μm pore size organic microfiltration membrane,then the target compounds were detected by fluorescence detector at an excitation wavelength of 248 nm and an emission wavelength of 447 nm while the flow cell was constant at 45℃,and then determined by external standard method.The experimental results indicated that,acridine showed a good relationship within the range of 2 pg to 2μg(R2=0.9999),the limit of detection was 0.083μg/L,the limit of quantification was 0.275μg/L,the analytical time was 12 min,and the recoveries of spiked concentrations of 1μg/L,10μg/L and 100μg/L were between 47%to 130%with a relative standard deviation of 0.5%to 2.0%.This method was simple,accurate,sensitive,and had low detection input,which was suitable for daily detection in alcoholic beverage manufacturers.