摘要
目的:建立RP-HPLC法同时测定不同规格鹿茸片中15种氨基酸的含量,根据氨基酸的含量对鹿茸片进行质量评价和等级区分。方法:样品以异硫氰酸苯酯进行柱前衍生化;采用C18色谱柱(250 mm×4.6mm,5μm),以0.1mol·L-1醋酸钠(醋酸调pH至6.5)-乙腈(93∶7)为流动相A,乙腈-水(4∶1)为流动相B,梯度洗脱,柱温为43℃,检测波长为254 nm。结果:15种氨基酸线性方程相关系数均大于0.999 4,平均回收率均在96.9%~103.2%,RSD均小于3.0%;50批样品中,蜡片中氨基酸含量最高,含量为44.56%~54.09%;骨片氨基酸含量最低,含量为29.53%~33.95%;粉片氨基酸含量为40.00%~45.33%,血片氨基酸含量为32.88%~39.96%。结果表明等级高的鹿茸片中氨基酸含量高于等级低的鹿茸片中氨基酸含量。结论:该方法可用于鹿茸饮片氨基酸的含量测定及为不同规格鹿茸饮片的质量等级评价提供数据支持和理论依据。
Objective:To establish an RP-HPLC method for simultaneous determination of 15 amino acids in deer velvet slices of different specifications,and carry out the quality evaluation and grade differentiation of deer velvet slices according to the contents of amino acids. Methods:The samples were derivated with phenyl isothiocyanate(PITC) pre-column and gradiently eluted with the mobile phase A(0.1 mol·L-1 sodium acetate buffer solution(p H adjusted to 6.5 with acetic acid)) and the mobile phase B[acetonitrile-water(4∶1)]. The column temperature was 36℃ and the detection wavelength was 254 nm. Results:The correlation coefficients of the linear equation of 15 amino acids were all above 0. 9994 and the average recoveries ranged from 96.9% to 103.2% with RSDs below 3.0%. Among the 50 batches samples,the amino acid contents of the wax slices were the highest and the contents were 44.56%-54.09%. While those of the bone slices were the lowest and the contents were 29.53%-33.95%. The amino acid contents of powder slices were 40.00%-45.33%,and the amino acid contents of blood slices were 32.88%-39.96%. The results showed that amino acid contents of high grade deer velvet slices was higher than that of low grade deer velvet slices. Conclusion:The method can be used for determining the amino acid contents of deer velvet slices and provide data support and theoretical basis for evaluating the quality grade of different specifications of deer velvet slices.
作者
郭晓晗
程显隆
柳温曦
李明华
魏锋
马双成
GUO Xiao-han;CHENG Xian-long;LIU Wen-xi;LI Ming-hua;WEI Feng;MA Shuang-cheng(National Institutes for Food and Drug Control,Beijing 100050,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2020年第10期1780-1789,共10页
Chinese Journal of Pharmaceutical Analysis
基金
重大新药创制“中药安全检测技术及标准平台”(2014ZX09304307-002)
国家自然科学基金“基于特征肽段智能识别的鹿茸及相关产品真伪鉴别系统研究”(81773856)
学科带头人培养基金鹿茸及相关产品真伪鉴别系统(2015X8)。