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目的建立冬枣中糖精钠的高效液相色谱测定方法。方法取果肉部分,经过高速匀浆、超声提取和沉淀、离心处理,进样测定。采用Atlantis C18色谱柱,以甲醇-0.02 mol/L乙酸铵为流动相,在230 nm波长处检测,以外标法定量。结果糖精钠的浓度为1.00μg/ml~50.0μg/ml时,线性关系良好,线性回归方程为y=4.42×10-4x+6.08×103,相关系数(r)=0.999 5。取20 g匀浆(大约相当于取12 g原始样品)测定时,方法的检出限为1.0×10-4g/kg,定量限为3.3×10-4g/kg。在低、中、高3种加标浓度下的回收率为92.0%~100.0%,中等浓度下平行测定6次的相对标准偏差(RSD)为1.9%~2.4%。结论该法操作简单,线性范围宽,精密度和回收率均满足方法学要求。
Objective To establish a method for the determination of saccharin sodium in winter jujube by high performance liquid chromatography. Methods Take the pulp part, after high-speed homogenization, ultrasonic extraction and precipitation, centrifugation, injection determination. An Atlantis C18 column with methanol-0.02 mol / L ammonium acetate as mobile phase was used to determine the absorbance at 230 nm and was quantified by external standard method. Results When the concentration of sodium saccharin was 1.00μg / ml ~ 50.0μg / ml, the linear relationship was good. The linear regression equation was y = 4.42 × 10-4x + 6.08 × 103, and the correlation coefficient (r) was 0.999 5. The method has a detection limit of 1.0 × 10-4g / kg and a limit of quantification of 3.3 × 10-4g / kg when taking 20g of homogenate (equivalent to approximately 12g of the original sample). The recoveries were 92.0% -100.0% at low, medium and high spiked concentrations, and from 1.9% to 2.4% at 6 replicates at moderate concentrations. Conclusion The method is simple, linear range, precision and recovery meet the methodological requirements.