超高效液相色谱法在原料药和中间体分析中的应用研究
发布时间：2019-07-04 06:52
【摘要】：本文根据卡马西平药典方法建立超高效液相色谱法(UPLC)检测有关物质,重点考察了原料药卡马西平有关物质的分析方法的可行性,对方法进行了验证,考察了UPLC方法的专属性、检出限、定量限、精密度、线性范围、准确度、稳定性和耐用性。结果显示溶液稳定性、线性、定量限、检出限、准确度、精密度、专属性均符合要求,其中考察耐用性时,流速调整为0.2mL/min时分离度不符合要求,说明在实验检测时,应严格控制流速。根据实验结果,该UPLC方法可适用于卡马西平有关物质的检测,与传统高效液相色谱法(HPLC)方法相比,检测时间从80分钟缩短到23分钟,大大提高了检测效率。建立了中间体2-氯-4-(二甲基砜)嘧啶(NAMD)的有关物质UPLC分析方法,并考察了NAMD分析方法的灵敏度和溶液稳定性。结果表明样品在乙腈:水=1:1为溶剂,室温条件下很不稳定,冷藏条件下2小时内稳定性较好。故样品溶液须冷藏,并及时进行检测。通过对中间体2,4-二氯嘧啶(NAMD05)和2-氯-4-(甲硫基)嘧啶(NAMD10)色谱纯度分析方法的筛选,实验和结果,建立了NAMD05和NAMD10色谱纯度UPLC分析方法,该方法运行时间8分钟,达到了高效检测的目的。同时通过方法学研究,考察NAMD05和NAMD10分析方法的灵敏度;NAMD10供试溶液在乙腈:水=1:1为溶剂,室温条件下的稳定性,为有效控制NAMD05和NAMD10的质量提供了依据。
[Abstract]:In this paper, an ultra-high performance liquid chromatography (HPLC) (UPLC) method for the determination of related substances was established according to carbamazepine Pharmacopoeia. The feasibility of the analytical method of carbamazepine was investigated. The method was verified. The specificity, detection limit, quantitative limit, precision, linear range, accuracy, stability and durability of the UPLC method were investigated. The results show that the stability, linearity, quantitative limit, detection limit, accuracy, precision and specificity of the solution all meet the requirements. When the durability is investigated, the separation degree does not meet the requirements when the flow rate is adjusted to 0.2mL/min, which indicates that the flow rate should be strictly controlled in the experimental test. According to the experimental results, the UPLC method can be applied to the detection of carbamazepine related substances. Compared with the traditional high performance liquid chromatography (HPLC) (HPLC) method, the detection time is shortened from 80 minutes to 23 minutes, which greatly improves the detection efficiency. A UPLC method for the determination of intermediate 2-chloro-4-(dimethyl sulfone) pyrimidine (NAMD) was established, and the sensitivity and solution stability of the NAMD method were investigated. The results show that the sample is unstable at room temperature and stable within 2 hours under cold storage when the solvent of acetonitrile: water = 1:1 is used as solvent. Therefore, the sample solution should be refrigerated and tested in time. Through the screening of chromatographic purity analysis methods of intermediates 2, 4-dichloropyrimidine (NAMD05) and 2-chloro-4-(methylthiopyrimidine) (NAMD10), NAMD05 and NAMD10 chromatographic purity UPLC analysis methods were established. The method runs for 8 minutes and achieves the purpose of high efficiency detection. At the same time, the sensitivity of NAMD05 and NAMD10 was investigated by methodological study, and the stability of NAMD10 solution at room temperature was studied under the condition of acetonitrile: water = 1:1, which provided the basis for effectively controlling the quality of NAMD05 and NAMD10.
【学位授予单位】：浙江工业大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O657.72;TQ460.7
[Abstract]:In this paper, an ultra-high performance liquid chromatography (HPLC) (UPLC) method for the determination of related substances was established according to carbamazepine Pharmacopoeia. The feasibility of the analytical method of carbamazepine was investigated. The method was verified. The specificity, detection limit, quantitative limit, precision, linear range, accuracy, stability and durability of the UPLC method were investigated. The results show that the stability, linearity, quantitative limit, detection limit, accuracy, precision and specificity of the solution all meet the requirements. When the durability is investigated, the separation degree does not meet the requirements when the flow rate is adjusted to 0.2mL/min, which indicates that the flow rate should be strictly controlled in the experimental test. According to the experimental results, the UPLC method can be applied to the detection of carbamazepine related substances. Compared with the traditional high performance liquid chromatography (HPLC) (HPLC) method, the detection time is shortened from 80 minutes to 23 minutes, which greatly improves the detection efficiency. A UPLC method for the determination of intermediate 2-chloro-4-(dimethyl sulfone) pyrimidine (NAMD) was established, and the sensitivity and solution stability of the NAMD method were investigated. The results show that the sample is unstable at room temperature and stable within 2 hours under cold storage when the solvent of acetonitrile: water = 1:1 is used as solvent. Therefore, the sample solution should be refrigerated and tested in time. Through the screening of chromatographic purity analysis methods of intermediates 2, 4-dichloropyrimidine (NAMD05) and 2-chloro-4-(methylthiopyrimidine) (NAMD10), NAMD05 and NAMD10 chromatographic purity UPLC analysis methods were established. The method runs for 8 minutes and achieves the purpose of high efficiency detection. At the same time, the sensitivity of NAMD05 and NAMD10 was investigated by methodological study, and the stability of NAMD10 solution at room temperature was studied under the condition of acetonitrile: water = 1:1, which provided the basis for effectively controlling the quality of NAMD05 and NAMD10.
【学位授予单位】：浙江工业大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O657.72;TQ460.7
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