【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(cè)有關(guān)物質(zhì),重點(diǎn)考察了原料藥卡馬西平有關(guān)物質(zhì)的分析方法的可行性,對(duì)方法進(jìn)行了驗(yàn)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(zhǔn)確度、穩(wěn)定性和耐用性。結(jié)果顯示溶液穩(wěn)定性、線性、定量限、檢出限、準(zhǔn)確度、精密度、專屬性均符合要求,其中考察耐用性時(shí),流速調(diào)整為0.2mL/min時(shí)分離度不符合要求,說明在實(shí)驗(yàn)檢測(cè)時(shí),應(yīng)嚴(yán)格控制流速。根據(jù)實(shí)驗(yàn)結(jié)果,該UPLC方法可適用于卡馬西平有關(guān)物質(zhì)的檢測(cè),與傳統(tǒng)高效液相色譜法(HPLC)方法相比,檢測(cè)時(shí)間從80分鐘縮短到23分鐘,大大提高了檢測(cè)效率。建立了中間體2-氯-4-(二甲基砜)嘧啶(NAMD)的有關(guān)物質(zhì)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(jié)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(shí)內(nèi)穩(wěn)定性較好。故樣品溶液須冷藏,并及時(shí)進(jìn)行檢測(cè)。通過對(duì)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(shí)驗(yàn)和結(jié)果,建立了NAMD05和NAMD10色譜純度UPLC分析方法,該方法運(yùn)行時(shí)間8分鐘,達(dá)到了高效檢測(cè)的目的。同時(shí)通過方法學(xué)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(zhì)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(xué)位授予單位】：浙江工業(yè)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：O657.72;TQ460.7

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