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目的建立一种高效液相色谱法测定面条中柠檬黄和日落黄含量的不确定度分析方法。方法选用无水乙醇-氨水-水(7:2:1)为样品的提取溶剂,色谱柱为Waters SymmetryC18柱(250 mm×4.6 mm,5μm),流速1.0mL·min-1,柱温:35℃,流动相以甲醇为A相,以含0.02 moL·L-1乙酸铵溶液、1%冰醋酸和0.2%三乙胺的水溶液(pH=4)为B相,进行梯度洗脱,考查实验过程中对含量的测定有影响的所有因素,确定不确定度来源,建立结果数学模型,计算各个不确定度分量,从而合成不确定度。结果拟合标准曲线过程中产生的不确定度最大,其次是样品处理过程中产生的不确定度,仪器产生的不确定度最小。结论本方法客观、准确,适用于高效液相色谱法测定面条中柠檬黄和日落黄含量的不确定度计算,也可用于计算含量实验方法的不确定度,在实际工作中有较强的实用性。
OBJECTIVE To establish an HPLC method for the determination of yellow lemon yellow and sunset yellow noodles uncertainty analysis method. Methods The extraction solvent was ethanol-ammonia-water (7: 2: 1). The column was a Waters Symmetry C18 column (250 mm × 4.6 mm, 5 μm) with a flow rate of 1.0 mL · min- : 35 ℃, the mobile phase is methanol, phase A, gradient elution is carried out with the aqueous phase containing 0.02 mol·L-1 ammonium acetate solution, 1% glacial acetic acid and 0.2% triethylamine as the phase B, Examining all the factors influencing the determination of the content during the experiment, determining the source of the uncertainty, establishing the mathematic model of the result, calculating the components of each uncertainty to synthesize the uncertainty. Results The uncertainty in fitting the standard curve was the highest, followed by the uncertainty in sample processing, and the least uncertainty in the instrument. Conclusion The method is objective and accurate and can be applied to the determination of the uncertainty of yellow and yellow in noodles by HPLC. It can also be used to calculate the uncertainty of experimental methods, which is more practical in practical work Sex.