摘要
建立同时测定兽用消毒剂枸橼酸苹果酸粉中枸橼酸和苹果酸含量的高效液相色谱方法。采用Agilent Eclipse XDB-C18(250mm×4.6mm,5μm)色谱柱,以乙腈-10mL/L磷酸溶液(2.5∶97.5,V/V)为流动相进行洗脱,流速为1.0mL/min,检测波长为210nm,柱温为35℃,进样量为20μL。枸橼酸和苹果酸色谱峰分离度良好。枸橼酸和苹果酸分别在100μg/mL^1 000μg/mL和50μg/mL^500μg/mL范围内线性关系良好。精密度、稳定性和重现性等考察结果的相对标准偏差(RSD)均小于1.0%;而平均回收率均在98%~101%之间,RSD均小于0.5%,符合方法学要求。6份供试品中枸橼酸和苹果酸的含量也均符合要求。建立的高效液相色谱法能够同时定量测定枸橼酸和苹果酸的含量,可用于枸橼酸苹果酸粉的质量控制。
To establish a HPLC method for simultaneous determination of citric acid and malic acid in citric acid and malic acid powder,the assay was conducted on an agilent eclipse XDB-C18 column(250mm×4.6mm,5μm) with acetonitrile-10 mL/L H3PO4 solution (2.5 :97.5,V/V). The flow rate was 1.0 mL/min, the detection wavelength was 210 nm, the column temperature was 35℃ and the injection volume was 20 μL. The results showed good resolution for the chromatographic peaks of citric acid and malic acid. The correlation coefficient between concentration and chromatographic peak area was over 0. 999 in the range of 100-1 000μg/mL for citric acid and 50-500 μg/mL for malic acid,indicating the good linearity of the calibration curves. In the precision,stability and repeated experiments, the relative standard deviations of citric acid and malic acid were less than 1.0%, showing a satisfactory precision and stability of this method. In the spiked experiment of three levels, the average recovery of citric acid and malic acid was about 98%- 101% and all the relative standard deviations were less than 0.5%, demonstrating that this method was considerably accurate. This HPLC method can be used for the quantitative determination of citric acid and malic acid simultaneously and the quality control in citric acid and malic acid powder.
出处
《动物医学进展》
北大核心
2017年第4期75-79,共5页
Progress In Veterinary Medicine