液液萃取/高效液相色谱法测定豆干与腐竹中溶剂黄2及溶剂黄56

Determination of Solvent Yellow 2 and Solvent Yellow 56 in Dried Bean Curd and Yuba by Liquid-Liquid Extraction/High Performance Liquid Chromatography

建立了液液萃取/高效液相色谱法测定豆干和腐竹中溶剂黄2和溶剂黄56的分析方法。样品经乙腈饱和的正己烷提取后,加入正己烷饱和的乙腈萃取,将乙腈层转入浓缩瓶内,重复萃取3次,将萃取液浓缩后用乙腈定容。采用Agilent TC-C18（4.6 mm×250 mm,5μm）色谱柱对样品进行分离;柱温为30℃;流动相为水-甲醇（20∶80）;流速为1.0 m L/min;检测波长为410 nm。溶剂黄2和溶剂黄56在0.30~50 mg/L浓度范围内线性关系良好,其检出限（LOD）和定量下限（LOQ）分别均为0.15 mg/kg和0.50 mg/kg,方法的平均回收率为85.4%~94.6%,相对标准偏差（RSD,n=6）为0.3%~2.3%。该方法重复性好,灵敏度高,适用于豆干和腐竹中溶剂黄2和溶剂黄56含量的测定。

A method for the determination solvent yellow 2 and solvent yellow 56 in dried bean curd and yuba was developed using liquid- liquid extraction- high performance liquid chromatography（ LLE- HPLC）. The samples were extracted by ultrasonic using hexane saturated with acetonitrile.Then,the target compounds were vortex extracted using acetonitrile saturated with hexane. The acetonitrile was moved into concentrated bottle. Operation steps were repeated for three times. The extraction solution was kept in constant volume after concentration. The concentrated solution was tested by high performance liquid chromatography. The target compounds were separated on a TC- C18（ 4. 6mm × 250 mm,5 μm） column using water- methanol（ 20 ∶ 80） as mobile phase at a flow rate of1. 0 m L/min. The column temperature was set at 30 ℃,and the detection wavelength was 410 nm.Under the optimal conditions,the calibration curves of solvent yellow 2 and solvent yellow 56 were linear in the range of 0. 30- 50 mg/L. The limits of detection（ LOD） of two targets compounds were both 0. 15 mg/kg,and the limits of quantitation（ LOQ） were both 0. 50 mg/kg. The average spiked recoveries of two target compounds in dried bean curd and yuba were in the range of 85. 4%-94. 6%,with relative standard deviations（ RSD,n = 6） of 0. 3%- 2. 3%. With good repeatability and high sensitivity,the method was suitable for the determination solvent yellow 2 and solvent 56 in dried bean curd and yuba samples.