高效液相色谱法测定炔丙基半胱氨酸及其有关物质的含量  

Determination of S-propargylcysteine and its related substances by high perfor-mance liquid chromatography

作　　者：徐琛[1] 陈益乐[1] 赵志鹏[2] 吕燕平[1] 段更利[1] 郁颖佳[1] 

机构地区：[1]复旦大学药学院药物分析教研室,上海201203 [2]同济大学经济与管理学院,上海200092

出　　处：《中国新药与临床杂志》2012年第6期308-311,共4页Chinese Journal of New Drugs and Clinical Remedies

摘　　要：目的建立高效液相色谱法测定炔丙基半胱氨酸(SPRC)及有关物质的含量。方法采用Welchrom-AQ C18色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈-离子对缓冲液(10 mmol.L-1庚烷磺酸钠+20 mmol.L-1KH2PO4,H3PO4调pH至2.4)(10∶90,V/V),紫外检测波长210 nm,流速1.0 mL.min-1。结果 SPRC在5.0～25.0 mg.L-1范围内具有良好的线性关系(r=0.999 5),最低检测限0.2 mg.L-1;样品溶液在24 h内稳定,精密度良好(<1.0%),回收率在98.0%～100.0%之间,3批样品的标示百分含量分别为96.94%、96.67%和96.56%,有关物质的含量分别为3.20%、3.43%和3.65%。结论本方法简便、灵敏,结果可靠准确,可用于SPRC及其有关物质的含量测定。AIM To establish a HPLC method for the quality control of S-propargylcysteine （SPRC） and its related substances. METHODS The separation was performed on a Welchrom-AQ C18 column （4.6 mm × 250 mm, 5 μm）. The mobile phase consisted of acetonitrile and ion buffer （10 mmol·L^-1 heptane sulfonate ＋ 20 mmol·L^-1 KH2PO4, pH was adjusted to 2.4 by phosphoric acid） （10 ： 90, V/V）. The flow rate was 1.0 mL·min^-1. The UV detection was set at 210 nm. RESULTS The assay showed good linear correlation over the range of 5.0 - 25.0 mg· L^-1（r = 0.999 5）. The limit of detection of SPRC was 0.2 mg·L^-1. The sample solution was stable in 24 h. The RSD were less than 1.0%. The average recovery of the method was between 98.0% - 100.0%. The content of SPRC in three batches of samples was 96.94%, 96.67%, and 96.56%. And the content of related substance was 3.20%, 3.43%, and 3.65%, respectively. CONCLUSION This method is rapid, simple, sensitive and accurate with valuable application to the quality control of SPRC and its related substances.

关 键 词：炔丙基半胱氨酸 色谱法 高效液相 有关物质 大蒜 

分 类 号：R917[医药卫生—药物分析学]