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食品研究与开发:2022,43(20):172-178
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不同衍生剂柱前衍生-HPLC-SPD二极管阵列测定特殊医学用途配方粉中牛磺酸含量
(1.湖南省产商品质量检验研究院,湖南 长沙 410000;2.食品安全监测与预警湖南省重点实验室,湖南 长沙 410000)
Determination of Taurine in Formula Powder for Special Medical Use by Pre-column Derivatization-HPLC with SPD Diode Array
(1.Hunan Provincial Institute of Product and Goods Quality Inspection,Changsha 410000,Hunan,China;2.Hunan Provincial Key Laboratory of Food Safety Monitoring and Early Warning,Changsha 410000,Hunan,China)
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投稿时间:2021-08-03    
中文摘要: 考察3种不同衍生剂的衍生效果,建立柱前衍生-高效液相色谱-SPD二极管阵列对特殊医学用途配方粉中牛磺酸含量的检测方法。特殊医学用途配方粉经温水溶解,超声辅助提取,以乙酸铵溶液(pH4.2)-乙腈作为流动相,采用 2,4-二硝基氟苯(2,4-dinitrofluorobenzene,DNFB)、丹磺酰氯(dansulfonyl chloride,Dansyl-Cl)、邻苯二甲醛(O-phthalaldehyde,OPA)3种不同衍生剂对其进行柱前衍生,用高效液相色谱-SPD二极管阵列进行测定。从样品检测总时长、操作步骤、回收率、样品稳定性及准确性多角度考察这3种不同衍生剂对牛磺酸含量测定的影响。结果表明:牛磺酸含量在浓度为2.01 μg/mL~60.30 μg/mL的范围内线性关系好,相关系数均达0.999以上,在20、40、80 mg/100 g的加标水平下,回收率为94.4%~103.7%,3种衍生剂均能满足特殊医学用途配方粉中牛磺酸的测定,实际样品检测结果差异不大;从整个检测分析过程看,3种不同衍生剂的衍生方式适合程度依次为2,4-二硝基氟苯>丹磺酰氯>邻苯二甲醛。
Abstract:The derivatization effects of three different derivatization agents were investigated,and a method of pre-column derivatization-high performance liquid chromatography with SPD diode array was established for the determination of taurine in formula powder for special medical use.The formula powder was dissolved in warm water and extracted with ultrasound.The extract was pre-column derivatized with 3 different agents:2,4-dinitrofluorobenzene(DNFB),dansulfonyl chloride(Dansyl-Cl),and O-phthalaldehyde(OPA).The high performance liquid chromatography with SPD diode array was conducted with ammonium acetate solution(pH4.2)-acetonitrile as the mobile phase.The effects of the three derivatizing agents on the determination of taurine were investigated from total detection time,operation steps,recovery rate,sample stability,and accuracy.The results showed that within the taurine concentration range of 2.01 μg/mL-60.30 μg/mL,the linear relationship was good,with the correlation coefficients all above 0.999.The recovery rates ranged from 94.4% to 103.7% at the spiked levels of 20,40 and 80 mg/100 g.The three derivatizing agents met the requirements for the determination of taurine in formula powder for special medical use,and the determination results had no significant difference from that in the real samples.Considering the whole detection and analysis process,the suitability of the three derivatizing agents were DNFB>Dansyl-Cl>OPA.
文章编号:202220022     中图分类号:    文献标志码:
基金项目:湖南省市场监督管理局科技计划项目(2021KJJH49)
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