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HPLC法测定磷酸替米考星可溶性粉中替米考星含量的研究 |
马春芳,李敏,张雯,吴春燕,陈建蓉,邓亚婷,王旗,余永涛,杨奇 |
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(宁夏兽药饲料监察所) |
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摘要: |
目的 建立磷酸替米考星可溶性粉中替米考星含量测定方法。方法 采用高效液相色谱(HPLC)法,使用十八烷基硅烷键合硅胶为填充剂的色谱柱,以水:乙腈:磷酸二丁胺缓冲液:四氢呋喃(805:115:25:55)为流动相,流速为1.0 mL/min,检测波长为280 nm,柱温为25℃。按外标法以峰面积计算含量。结果 在此色谱条件下,替米考星顺式、反式异构体峰分离度良好,磷酸替米考星可溶性粉的线性范围在0.05~1 mg/mL内r2﹥0.9999,平均回收率为97.96%,RSD<1.0%。结论 本研究建立的方法分离效果好、精密度高、稳定性好,能作为磷酸替米考星可溶性粉的质量关键控制指标。 |
关键词: 磷酸替米考星可溶性粉,高效液相色谱法 替米考星,含量测定 |
DOI: |
投稿时间:2020-07-06修订日期:2021-02-04 |
基金项目:宁夏回族自治区重点研发计划项目“畜禽产品质量安全评价与监控技术应用研究”(编号:2018BBF02002) |
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Study on the Determination Method of Tilmicosin Content in Soluble Powder of Timicostar phosphate |
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(Ningxia Veterinary Drugs and Administration) |
Abstract: |
Objective To establish a method for the determination of temicostar in phosphate soluble powder. Methods HPLC was used for the column with octadecyl silane bonded silica gel as the filler,and the mobile phase was determined with water: acetonitrile: dibutylamine phosphate solution: tetrahydrofuran (805:115:25:55); The flow rate was 1.0 mL/min, the detection wavelength was 280 nm, and the column temperature was 25℃.Calculate content by peak area according to external standard method. Results Under these chromatographic conditions, the separation of cis - and trans - isomers was satisfactory. The linear range of timicoxacin phosphate soluble powder was 0.05 ~ 1 mg/mL, r2 > 0.9999. The average recovery was 97.96%, RSD < 1.0%. Conclusion The method established in this study has good separation effect, high precision and good stability, and can be used as a key quality control index for the soluble timicoxacin phosphate powder. |
Key words: Temicol phosphate soluble powder, High performance liquid chromatography, content |