柱前衍生-高效液相色谱法测定肠内营养剂中脯氨酸的含量  被引量:2

Pre-column derivatization-HPLC method for determination of proline in enteral nutrition

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作  者:徐倩昱[1] 蔡熠[1] 陈斌[1] 徐琛[1] 郁颖佳[1] 李嫣[1] 段更利[1] 

机构地区:[1]复旦大学药学院药物分析教研室,上海201203

出  处:《中国临床药学杂志》2011年第6期362-364,共3页Chinese Journal of Clinical Pharmacy

摘  要:目的建立一种柱前衍生-高效液相色谱法测定肠内营养剂中脯氨酸的含量。方法以氯甲酸-9-芴基甲酯(FMOC-Cl)为衍生化试剂,色谱柱采用Agilent C_(18)(150 mm×4.6 mm,5.0μm)柱,流动相为乙腈-50 mmol·L^(-1)醋酸钠缓冲液(pH4.2),梯度洗脱,流速为1.0 mL·min^(-1),柱温30℃;FLD荧光检测,激发波长263 nm,发射波长315nm。待测肠内营养剂样品经10 mol·L^(-1)盐酸溶液溶解稀释后,超声提取,在室温条件下与衍生化试剂反应15 min,反应终止并取20μL进样分析。结果脯氨酸在质量浓度0.1~1 mg·L^(-1)内线性关系良好,r=0.999 6;平均回收率109.42%~112.72%,日间、日内精密度RSD均<7%;样品溶液在24 h内稳定。结论该方法灵敏、简便、专属性强,能对肠内营养剂中的脯氨酸进行准确的定量分析,并能避免制剂中其他氨基酸组分的干扰。AIM To develop a pre-column derivatizafion-HPLC method for the detemaination of proline in enteral nutrition. METHODS AnAgilent Clscolumn (150mmx4.6mm, 5.0ptm) was used with a mobile phase consisting of acetonitrile-sodimn acetate (pH 4.2, 50 mmol'L-1) for gradient elution analysis. The flow rate was 1.0 mL'min-:. The column temperature was 30~C. The ~x of ~ was 263 nm and the ?'era Was 315 rim. The derivatization reagent was 9-fluorenylmethyl chloroformate (FMOC-C1). RESULTS The linear range of proline was 0.1 - 1 rng" L-i( r = 0.999 6). The range of average recoveries was 109.42% - 112.72%. Both the inter-day RSD and the intra-day RSD were less than 7 %. The sample solvent was stable in 24 h. CONCLUSION The method is simple, sensitive and spe- cific which can be applied for determination of proline in enteral nutrition and for quality control of the preparation.

关 键 词:脯氨酸 氯甲酸-9-芴基甲酯 柱前衍生-高效液相色谱 肠内营养剂 

分 类 号:R927.2[医药卫生—药学]

 

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