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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
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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.
出处 《中国新药与临床杂志》 CAS CSCD 北大核心 2012年第6期308-311,共4页 Chinese Journal of New Drugs and Clinical Remedies
关键词 炔丙基半胱氨酸 色谱法 高效液相 有关物质 大蒜 S-propargylcysteine chromatography, high pressure liquid related substances garlic
作者简介 徐琛(1988-),女,上海人,硕士研究生,主要从事药物分析研究 [责任作者]郁颖佳,Phn:86-21-5198-0052,E-mail:yuyj@fudan.edu.cn
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参考文献9

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