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吡硫醇锌检测方法的建立

论文编号:HG181 论文字数: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(10mmolL 磷酸二氢钾和0. 5mmoll 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. 5mmoll 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

吡硫醇锌检测方法的建立......