亚硝化衍生超高效液相色谱法测定酱腌菜中亚硝酸盐的含量

Determination of nitrite content in pickles by nitroso derivative ultra performance liquid chromatography

中文关键词:  亚硝酸盐,酱腌菜,超高效液相色谱法,安替比林

英文关键词:nitrite  pickles  ultra performance liquid chromatography  antipyrin

中文摘要:

      目的 建立亚硝化衍生超高效液相色谱法测定酱腌菜中亚硝酸盐含量的方法。方法 在0.02 mol/L乙酸铵缓冲液(内含0.1%乙酸)中, 安替比林与亚硝酸盐相互作用, 生成亚硝基衍生物, 该衍生物在波长345 nm有较强的吸收, 用超高效液相色谱法进行检测分析, 采用ACQUITY UPLC BEH Shield RP18色谱柱(150 mm× 2.1 mm, 1.7 μm)进行分离, 外标法定量。结果 目标物在0.05~5.00 μg/mL质量浓度范围线性良好, 检出限为0.01 mg/L。高、中、低3水平浓度加标, 检测回收率为88%~96% (n=6), 相对标准偏差为2.0%~4.5%。结论 该方法能够有效消除氯离子等阴离子和色素对本研究的干扰, 建立的分析方法灵敏度、准确度、精密度和回收率好, 适用于酱腌菜中亚硝酸盐的测定。

英文摘要:

      Objective To establish a method for the determination of nitrite content in pickles by nitroso derivative ultra performance liquid chromatography. Methods A novel and sensitive method for the determination of nitrite content was developed. This is a nitroso derivative produced based on the interaction between nitrite and antipyrine This derivative has strong absorption in 0.02 mol/L acetate buffer solution (contains 0.1% acetic acid) at a wavelength of 345 nm the nitrite content was determined by ultra performance liquid chromatography. Results Nitrite in the linear concentration range of 0.05–5.00 mg/L was determined with a limit of detection 0.01 μg/mL. The high, medium and low concentrations were spiked. The extraction recoveries ranged from 88%–96% (n=6). The relative standard deviation was the precision ranged from 2.0%–4.5%. Conclusion The method can effectively eliminate the interference of chloride ions and other anions and pigments on this experiment. The established analytical method has good sensitivity, accuracy, precision and recovery rate, and is suitable for the detection of nitrite in pickles.