【摘要】：本文根據(jù)卡馬西平藥典方法建立超高效液相色譜法(UPLC)檢測有關物質,重點考察了原料藥卡馬西平有關物質的分析方法的可行性,對方法進行了驗證,考察了UPLC方法的專屬性、檢出限、定量限、精密度、線性范圍、準確度、穩(wěn)定性和耐用性。結果顯示溶液穩(wěn)定性、線性、定量限、檢出限、準確度、精密度、專屬性均符合要求,其中考察耐用性時,流速調(diào)整為0.2mL/min時分離度不符合要求,說明在實驗檢測時,應嚴格控制流速。根據(jù)實驗結果,該UPLC方法可適用于卡馬西平有關物質的檢測,與傳統(tǒng)高效液相色譜法(HPLC)方法相比,檢測時間從80分鐘縮短到23分鐘,大大提高了檢測效率。建立了中間體2-氯-4-(二甲基砜)嘧啶(NAMD)的有關物質UPLC分析方法,并考察了NAMD分析方法的靈敏度和溶液穩(wěn)定性。結果表明樣品在乙腈:水=1:1為溶劑,室溫條件下很不穩(wěn)定,冷藏條件下2小時內(nèi)穩(wěn)定性較好。故樣品溶液須冷藏,并及時進行檢測。通過對中間體2,4-二氯嘧啶(NAMD05)和2-氯-4-(甲硫基)嘧啶(NAMD10)色譜純度分析方法的篩選,實驗和結果,建立了NAMD05和NAMD10色譜純度UPLC分析方法,該方法運行時間8分鐘,達到了高效檢測的目的。同時通過方法學研究,考察NAMD05和NAMD10分析方法的靈敏度;NAMD10供試溶液在乙腈:水=1:1為溶劑,室溫條件下的穩(wěn)定性,為有效控制NAMD05和NAMD10的質量提供了依據(jù)。
[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.
【學位授予單位】：浙江工業(yè)大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：O657.72;TQ460.7

【參考文獻】

相關期刊論文 前10條

1 張學艷;;超高效液相色譜在西藥分析中的應用[J];黑龍江科技信息;2014年07期

2 ;沃特世推出涵蓋納升級至微升級的超高效液相色譜系統(tǒng)——ACQUITY UPLC M-Class[J];中國生物工程雜志;2014年02期

3 王超;彭濤;高愈霄;呂怡兵;滕恩江;;混合型固相萃取/超高壓液相色譜法測定廢水中苯胺類化合物[J];分析測試學報;2013年12期

4 林海丹;鄒志飛;秦燕;陳毓芳;李小麗;王嵐;劉中勇;;高效液相色譜法同時測定食品中18種食品添加劑[J];食品科學;2013年08期

5 孫文軍;杜振霞;于文蓮;周麗麗;;三相中空纖維液相微萃取/超高效液相色譜-串聯(lián)質譜法檢測飲品中的苯甲酸與山梨酸[J];分析測試學報;2012年12期

6 陳紅平;劉新;王川丕;尹鵬;;分散固相萃取-超高壓液相色譜-串聯(lián)質譜法測定茶葉中赤霉酸和α-萘乙酸[J];分析化學;2012年07期

7 李乾;靳s，

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