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刊物信息

期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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反相高效液相色谱与离子交换色谱测定牛肉中肌肽含量的对比研究

Comparative study on determination of carnosine in beef by RP-HPLC and IEC

作者(英文):
分类号:R917
出版年·卷·期(页码):2019,39 (5):805-812
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的:考察反相高效液相色谱(RP-HPLC)紫外检测与离子交换色谱(IEC)电导检测2种方法对牛肉中肌肽检测的一致程度。方法:RP-HPLC色谱条件:Agilent TC-C18色谱柱(5 μm,4.6 mm×250 mm);流动相为乙腈-水(15:85);柱温35℃;流速1.00 mL·min-1;进样体积25 μL;检测波长210 nm。IEC色谱条件:Dionex AminoPacTM PA-10(2 mm×50 mm)保护柱和Dionex AminoPacTM PA-10(2 mm×250 mm)分析柱分离,金电极检测,直流安倍电位,检测波形为"Amino Acids(Reference)"。以70%超纯水和30%醋酸钠溶液(100 mmol)为淋洗液;Dionex AminoPacTMPA-10柱流速为0.25 mL·min-1,进样体积均为25 μL。分别对2种方法的检测下限、精密度、加样回收率等进行考察,并对2种方法测得牛肉样品的结果进行显著性检验(F检验和t检验)。结果:RP-HPLC法线性范围为0.20~5.00 μg·mL-1R2=0.999 7),检测下限和定量下限分别为0.032和0.11 μg·mL-1,方法精密度(RSD)为1.2%(n=11),样品回收率为97.7%;IEC法峰形对称,线性范围为0.20~8.00 μg·mL-1R2=0.999 0),检测下限和定量下限分别为0.005 0和0.017 μg·mL-1,方法精密度(RSD)为1.2%(n=11),样品回收率为92.2%。对测定结果的F检验(方法精密度)表明两者无显著性差异,但t检验(方法系统误差)表明两者有显著差异。结论:2种方法均能较好地对样品中的肌肽进行定性和定量分析,但两者存在系统误差,原因需进一步探索。

-----英文摘要:---------------------------------------------------------------------------------------

Objective:To investigate the consistency of detecting carnosine in beef by reversed phase high performance chromatography (RP-HPLC) and ion exchange chromatography (IEC).Methods:RP-HPLC separation was accomplished on Agilent TC-C18 (5 μm, 4.6 mm×250 mm) column with mobile phase of acetonitrile-water (15:85) by flow rate of 1.00 mL·min-1 and the detection wavelength was 210 nm at 35℃. IEC separation was accomplished on Dionex AminoPacTM PA-10 (2 mm×50 mm) guard column and Dionex AminoPacTM PA-10 (2 mm×250 mm) analytical column with mobile phase of 70% ultrapure water-30% sodium acetate solution (100 mmol) by flow rate of 0.25 mL·min-1 and the detection wavelength was amino acids (reference) with amperometric detection on an a gold electrode. The detection limit, precision and sample recovery rate of the two methods were investigated, and the experiment results in beef samples were tested for significance (F-test and t-test).Results:RP-HPLC had good linearity in the range of 0.20-5.00 μg·mL-1 (R2 was 0.999 7), the limits of detection and quantification were 0.032 μg·mL-1 and 0.11 μg·mL-1 respectively, the precision (RSD) was 1.2% (n=11), and the sample recovery rate was 97.7%.The shape of IEC was symmetrical and had good linearity in the range of 0.20-8.00 μg·mL-1 (R2=0.999 0), the limits of detection and quantification were 0.005 0 μg·mL-1 and 0.017 μg·mL-1 respectively.The precision (RSD) was 1.2% (n=11), and the recovery was 92.2%.The F-test (precision of the methods) results showed there was no significant difference between the two methods.However, the t-test (systematic error of the methods) results showed there was significant difference between the two methods.Conclusion:The two methods can be used to qualitatively and quantitatively analyze carnosine in samples.However, there is systematic error between the two methods and the reasons need to be further explored.

-----参考文献:---------------------------------------------------------------------------------------

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