摘要
建立了硫辛酸片中硫辛酸及其降解物快速测定的高效液相色谱方法。采用Waters XBridge色谱柱(5μm,150 mm×4.6 mm),流动相为0.05 mol/L磷酸二氢钾溶液(磷酸调至pH 2.5)-乙腈-甲醇(50∶45∶5),流速为1.0 mL/min,进样量为20μL,二极管阵列检测器,检测波长为220 nm,全波长扫描范围为200～400 nm,柱温为室温。结果表明,在上述色谱条件下,硫辛酸浓度在0.4～20.0 mg/L范围内线性关系良好(r=0.999 9);其检出限为0.2 mg/L;定量下限为0.6 mg/L;精密度RSD(n=12)为3.4%;加标回收率为100.9%,RSD为2.0%。该法简便、快速、准确、选择性好、灵敏度高,可用于硫辛酸片含量与降解物的测定。
A high-performance liquid chromatographic（HPLC） method for the determination of relative substances in thioctic acid tablets was developed.The separation of analyte was performed on a Waters XBridge column（5 μm,150 mm×4.6 mm） with phosphate buffer（pH value was adjusted to 2.5 with phosphoric acid）-acetonitrile-methanol（50 ∶ 45 ∶ 5） as mobile phase,at a flow rate of 1.0 mL/min and an injection volume of 20 μL.The photo-diode array detector（PDA） was set at 220 nm,with full scan range of 200-400 nm.The column temperature was ambient.Under the above chromatographic conditions,the calibration curve was linear（r=0.999 9） in thioctic acid concentration range of 0.4-20.0 mg/L.The limit of detection（LOD） for thioctic acid was 0.2 mg/L and the limit of quantitation（LOQ） was 0.6 mg/L.The relative standard deviation（RSD,n=12） was 3.4%,and the average spiked recovery was 100.9% with RSD of 2.0%.The proposed method could be applied in the determination of relative substances in thioctic acid tablets with the advantages of simplicity,rapidity,accuracy,good selectivity and high sensitivity.
出处
《分析测试学报》
CAS
CSCD
北大核心
2013年第7期894-897,共4页
Journal of Instrumental Analysis
基金
广东省科技计划项目(2010A040209001)
关键词
硫辛酸片
硫辛酸
降解物
高效液相色谱法
thioctic acid tablet
thioctic acid
degradation products
HPLC
