论文总字数：17457字

摘 要

目的 建立甘草酸二铵肠溶胶囊中间体I中残留溶剂气相色谱定量分析方法。方法 通过优化固定相、进样方式和配制方法等条件，建立并评价了气相色谱方法：以6％氰丙基苯基-94％二甲基聚硅氧烷为固定液的毛细管柱，程序升温，初始温度60℃，以5℃·min^-1升至100℃，然后以35℃·min^-1升至230℃保持10分钟；柱流速为5mL·min^-1，载气为氮气；顶空进样；进样口温度200℃；检测器为FID，温度为260℃。结果 在上述分析条件下，各残留溶剂实现了基线分离；乙醇、乙酸乙酯分别在7.5～540μg·mL^-1、2.5～540μg·mL^-1的浓度范围内色谱响应呈线性，检测限分别为2.45μg·mL^-1、0.81μg·mL^-1。结论 所建方法重现性好，灵敏度和准确度均较高，可用于甘草酸二铵肠溶胶囊中间体I中残留溶剂定量分析。

【关键词】甘草酸二铵肠溶胶囊中间体I 气相色谱法 残留溶剂

abstract

objective Set up two ammonium glycyrrhetate enteric capsules in the intermediate I residual solvent gas chromatographic quantitative analysis method.Method by optimizing the stationary phase method, sampling method and preparation conditions, such as to establish and evaluate a method: gas chromatography with 6% cyanide propyl phenyl - 94% dimethyl polysiloxane stationary liquid capillary column, the program to heat up, the initial temperature of 60 ℃, in 5 ℃·min^-1 rose to 100 ℃, and then 35 ℃·min^-1 rose to 230 ℃ for 10 minutes;Column velocity is 5 ml·min^-1, carrier gas is nitrogen;Headspace sampling;Injection port temperature 200 ℃;To FID detector, temperature is 260 ℃.Results under the condition of the above analysis, the residual solvent has realized the baseline separation;Ethanol, ethyl acetate, respectively, in 7.5 ~ 540 μ g·mL ^{- 1}, 2.5 ~ 540 μg·mL ^{- 1} chromatographic response linear concentration range, detection limit were 2.45 μg·mL ^{- 1}, 0.81 μg· mL ^{- 1}.Conclusion the established method with good reproducibility, and have high sensitivity and accuracy, and can be used in the two ammonium glycyrrhetate enteric capsule intermediates I quantitative analysis of the residual solvents.

【key word】Diammonium Glycyrrhizinate Enteric-coated Capsules intermediate I; gas chromatography; residual solvent

目录

1. 文献综述....................................................................Ⅰ

1.1性质.....................................................1

1.2简介.....................................................1

1.3治疗与应用...............................................2

1.4甘草酸二铵处方及工艺.....................................3

1.4.1处方...............................................3

1.4.2仪器...............................................3

1.4.3载药微丸的制备.....................................4

1.4.4隔离微丸的制备.....................................4

1.4.5肠溶微丸的制备.....................................4

1.4.6其他剂型...........................................4

第二章 甘草酸二铵肠溶胶囊中间体Ⅰ残留溶剂定量分析方法的建立及应用研究...................................................6

2.1材料.....................................................6

2.1.1仪器................................................6

2.1.2试剂................................................6

2.1.3样品................................................6

2.2方法.....................................................6

2.2.1色谱条件............................................6

2.2.2标准溶液的配置......................................6

2.2.3供试品溶液的配置....................................6

2.2.4样品分析............................................7

2.3分析方法验证..............................................7

2.3.1专属性试验..........................................7

2.3.2精密度..............................................8

2.3.3检测限与定量限......................................9

2.3.4线性及范围..........................................9

2.3.5准确度..............................................9

2.3.6耐用性..............................................10

2.4分析方法结果.............................................11

2.4.1专属性..............................................11

2.4.2系统精密度..........................................11

2.4.3方法精密度..........................................11

2.4.4中间精密度..........................................11

2.4.5最小检测限（LOD）...................................12

2.4.6方法定量限（LOQ）...................................12

2.4.7线性和范围..........................................12

2.4.8准确度..............................................12

2.4.9耐用性..............................................13

2.5讨论......................................................13

2.5.1色谱柱的选择........................................13

2.5.2线性范围的选择......................................13

参考文献................................................14

致谢....................................................17

1. 文献综述

1.1性质

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