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高效液相色谱法测定卡巴匹林钙可溶性粉中卡巴匹林钙和游离水杨酸的含量
林仙军
0
(浙江省兽药饲料监察所)
摘要:
建立了一种可同时测定卡巴匹林钙可溶性粉中卡巴匹林钙和游离水杨酸含量的高效液相色谱方法。采用Agilent Zorbax XDB C18 250 mm×4.6 mm,5 μm色谱柱,流动相为0.2%磷酸溶液-乙腈(70:30,v:v),流速1.0 mL/min,检测波长228 nm,柱温30 ℃。结果卡巴匹林钙和水杨酸在0.1~100 μg/mL浓度范围内线性关系良好相关系数r均大于0.999;卡巴匹林钙回收率为97.4%~101.1%,批内相对标准偏差为0.4%~1.3%,批间相对标准偏差为0.2%~0.5%;水杨酸回收率为96.9%~101.2%,批内相对标准偏差为0.5%~1.5%,批间相对标准偏差为0.2%~0.5%。方法操作简便、准确、可靠,可用于卡巴匹林钙可溶性粉的质量控制。
关键词:  卡巴匹林钙  水杨酸  可溶性粉  高效液相色谱  含量测定
DOI:
投稿时间:2017-01-03修订日期:2017-03-28
基金项目:浙江省“三农六方”科技协作项目(CTZB-F160728AWZ-SNY1-25A)
Determination of Carbasalate Calcium and Free Salicylic Acid in Carbasalate Calcium Soluble Powder byHPLC
(Zhejiang Province Supervisory Institute of Veterinary Drug and Feed)
Abstract:
A high performance liquid chromatography method was established for the determination of carbasalate calcium and free salicylic acid in carbasalate calcium soluble powder. Separation was performed on a reversed-phase Agilent Zorbax XDB C18 column. The mobile phase consisted of a mixture of 0.2% phosphoric acid solution and acetonitrile(70:30, v/v) . The detection wavelength was 228 nm, the flow rate was 1.0 mL/min, and the column temperature was 30 ℃. A good linearity of the calibration curves was obtained with the range of 0.1~100 μg/mL for carbasalate calcium and free salicylic acid, the correlation coefficient r﹥0.999. The recoveries of carbasalate calcium were 97.4%~101.1%, the intra-assay coefficient of variation were 0.4%~1.3%, and the inter-assay coefficients of variation were 0.2%~0.5%. The recoveries of free salicylic acid were 96.9%~101.2%, the intra-assay coefficient of variation were 0.5% ~ 1.5%, and the inter-assay coefficients of variation were 0.2% ~ 0.5%. The method is simple, accurate and reliablein the determination of carbasalate calcium and free salicylic acid in carbasalate calcium soluble powder.
Key words:  carbasalate calcium  salicylic acid  soluble powder  HPLC  determination

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