摘要
目的:建立高效液相色谱-蒸发光散射检测法(HPLC-ELSD),直接测定疏血通注射液中17种未衍生氨基酸含量的方法。方法:以异亮氨酸等氨基酸为标准品;色谱柱:Prevail^(TM) C_(18)(4.6mm×250mm,5μm);流动相A:乙腈,流动相B:5.0mmol·L^(-1)七氟丁酸的0.7%三氟醋酸溶液,流动相A与B比例:0min为0∶100,5min为0∶100,8min为15∶85,25min为35∶65;漂移管温度:115℃;气体流量:2.5L·min^(-1);流速:0.8mL·min^(-1);柱温:35℃;进样量:10μL。结果:在25min内即可完成对疏血通注射液中17种氨基酸的分离测定,氨基酸质量浓度0.071～2.285g·L^(-1)时,其对数值与峰面积对数值线性关系良好,17种氨基酸的加样回收率为92.9%～105.1%,信噪比为3时,异亮氨酸检出限为20mg·L^(-1)。结论:该法不需要专门的氨基酸分析仪和衍生化氨基酸,操作简便,有足够的灵敏度,结果准确可靠。
Objective ：To establish an HPLC -ELSD method for determination of the 17 underivatized amino acids in Shuxuetong injection. Methods：The assay was conducted on a Prevail^TM C 18 column （4. 6 mm ×250mm,5μm） with isoleucine etc. as the standard substance. The 17 amino acids were separated within 25 min under the condition of gradient elution. The mobile phase A was acetonitrile, the mobile phase B was 5.0 mmol · L^- 1 heptafluorobutyric acid in 0. 7% trifluoroacetic acid solution. The ratios of the contents of mobile A and B were 0：100 at 0 min,0：100 at 5 min,15：85 at 8 min,35：65 at 25 rain. The detection was performed at the temperature of drift tube of 115 ℃ and the gas flow rate of 2. 5 L·min^-1. The flow rate was 0. 8 mL·min^-1, the column temperature was 35 ℃ and the inject volume was 10 μL. Results：The calibration curves were showed good linearity within the concentration range of 0. 071 -2. 285 g · L^-1. The average recoveries were 92.9% - 105.1%. While the signal - noise ratio was 3, the detection limit of isoleucine was 20 mg· L^-1. Conclusion：This method needs neither the special amino acid analyzer nor derivatizing amino acid, and is efficient, sensitive and accurate.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2007年第4期558-560,共3页
Chinese Journal of Pharmaceutical Analysis
