吡硫醇锌检测方法的建立

文档编号:HG181  文档字数:9522,页数:23

摘要：吡硫醇锌 (Pyrithionc Zinc, ZPT) 的分子量为317.7，外观是乳白色水分散体、灰白色粉末状固体，具有较强地杀真菌作用，外用治疗真菌感染，据报告用Z PT洗剂是很安全的。因局部可吸收部份药物 (0.05%—0 .8％ )；此外吡硫醇锌还有保鲜的效果。用 Z P T保鲜剂处理，可保持果实新鲜，好果率高，品质优良．可周年供应。
 本文主要采用高效液相色谱法对ZPT含量进行了检测，此方法简便、快速、结果可靠，可用于本品质量控制。实验采用:Diamonsil Cl8 柱 ,5 μm ,（250mm ×4.6mm)色谱柱，经改变流动相类型、配比、pH值等因素，确定最佳流动相配比为乙腈∶甲醇∶ 水溶液(10mmol\L 磷酸二氢钾和0. 5mmol\l L EDTANa2 ,磷酸调pH=4.14) = 50∶ 10∶ 40，流速1.0 ml/min，在检测波长230 nm下，得到标准曲线方程为Y=9299.5X-18030,R2=0.9997，加标回收率为101.90%，RSD为0.96%，精密度为0.13%。
关键词：高效液相色谱法（HPLC）；  ZPT；  吡啶硫酮铜络合物；  含量检测。

Abstract: The molecular weight of Pyrithionc Zinc is 317.7,  Appearance is a milky water spread、Gray solid. Having to kill a fungus role, With the treatment of fungal infection, Reported by z pt lotions is quite safe. For local can absorb some of the drug (0.05% - 0. 8 ％), The rich keep the sulphur is the effect of zinc. With z p t, can keep fresh fruit, fruit, high quality and can anniversary  provide.
   This article mainly adopt HPLC of zpt content of the testing . This method is simple, fast, reliable and can be validated to improve the quality control of ZPT. The chromatographic separation was performed on  a Diamonsil Cl8column(250 mm × 4.6 mm id, 5 μ m particle size). After several tests by changing the type of mobile phase, ratio and pH value, etc., a HPLC method using an elution with lAcetonitrile-Methano and 10mmol / L monopotassium phosphate and 0. 5mmol\l L EDTANa2  aqueous solution (pH=4.14, adjusted by phosphoric acid)( 50∶ 10∶40 ,V / V / V) at a flow-rate of 1.0 mL / min has been developed. At ultraviolet wavelength 230nm, the standard curve equation of zpt Y=9299.5X-18030, R2=0.9997, plus recovery of  101.90 percent , RSD to 0.96 %, precision of 0.13 % .
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 Key words:  high-performance liquid chromatography (HPLC); zinc pyrithione; Cu2+ complex of pyrithione  baicalin; Detection

 目 录
中文摘要 ...................................................................I
英文摘要 ..................................................................II
目录 ......................................................................Ⅲ
1. 绪论.....................................................................1
 1.1 ZPT简介............................................1
 1.1.1 ZPT检测方法...............................................1
 1.2高效液相色谱法检测ZPT含量...........................4
2. 实验部分.................................................................5
 2.1 材料与实验仪器.........................................................5
 2.1.1  实验试剂与样品..................................................5
 2.1.2  实验仪器........................................................5
 2.2 ZPT的含量检测方法的建立...................6
 2.2.1 ZPT标准溶液配制...........................................6
  2.3 高效液相色谱法检测ZPT的含量..............6
 2. 3. 1  ZPT的溶解度. . . . . . .. . . . . . . . . . . . . . . . . . . . . . . . 6
 2.3.3 流动相种类、配比、pH值的选择...................................6
 2. 3. 4 最低检出限测定. . . . . . . . . . . .. . . . . . .. . . . . . . . . . . 7
 2.3.2 精密度试验.......................................................7
  2. 4高效液相色谱法铜盐络合法测 ZPT的含量..............................7
3. 结果与讨论...............................................................7
 3.1ZPT的含量检测方法的建立....................7
 3.1.1 检测波长的选择...................................................7
 3.1.2 流动相种类、配比、pH值的选择.......................................11
 3.2 ZPT含量结果分析.......................... 11
 3.2.1 标准曲线的制作..................................................11
 3.2.2精密度试验...................................................12
 3.2.3 加标回收率试验.................................................. 13
 3.2.4最低检出限测定......................................................13
4．总结与展望...............................................................14
致谢.......................................................................16
参考文献...................................................................18

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