發(fā)布時間：2018-02-26 14:55

  本文關(guān)鍵詞： 離子色譜 甲磺酸雷沙吉蘭 羥胺　出處：《中國藥學(xué)雜志》2017年20期 　論文類型：期刊論文

【摘要】：目的建立譜睿-在線固相萃取-離子色譜法測定甲磺酸雷沙吉蘭藥品中痕量羥胺殘留含量的分析方法,為臨床用藥的藥學(xué)安全性提供保障。方法樣品經(jīng)溶解后直接進樣,在六通進樣閥和色譜分離柱之間,引入含陽離子富集柱——IonPac CG12A的切換閥,在線消除甲磺酸雷沙吉蘭樣品基體,待羥胺完全轉(zhuǎn)移至IonPac CS12A柱上后,以乙腈/甲基磺酸溶液清洗Ion Pac CG12A,完成了痕量羥胺殘留含量的自動固相萃取-在線分析,安培檢測,外標(biāo)法定量。結(jié)果方法專屬性、耐用性良好,羥胺在0.04~3.75μg·mL~(-1)內(nèi)具有良好的線性,相關(guān)系數(shù)(r~2)為0.999 9,其檢出限為0.02μg·mL~(-1),定量限為0.04μg·mL~(-1)。方法精密度較好,平行實驗檢測結(jié)果相對標(biāo)準(zhǔn)偏差(RSD)小于5%;方法準(zhǔn)確度較高,加標(biāo)回收率介于94%~103%之間。結(jié)論本方法應(yīng)用于甲磺酸雷沙吉蘭中痕量羥胺的分離測定,靈敏度高,檢測結(jié)果準(zhǔn)確可靠。
[Abstract]:Objective to establish a method for the determination of trace hydroxylamine residues in resagilan mesylate by spectral Rui on-line solid phase extraction (SPE) and ion chromatography, and to provide a guarantee for the pharmacological safety of clinical drugs. A cationic enriched column, IonPac CG12A switch valve, was introduced between the six way sample injection valve and the chromatographic separation column. The sample matrix of resagilan mesylate was eliminated on line, and the hydroxylamine was completely transferred to the IonPac CS12A column. Ion Pac CG12A was cleaned with acetonitrile / methyl sulfonic acid solution, and automatic solid phase extraction-on-line analysis, amperometric detection and external standard quantification of trace hydroxylamine were completed. The results showed that the method was specific and durable, and the hydroxylamine had a good linearity in the range of 0.04 ~ 3.75 渭 g 路mL ~ (-1). The correlation coefficient is 0.999 9, the detection limit is 0.02 渭 g 路mL ~ (-1) and the quantitative limit is 0.04 渭 g 路mL ~ (-1). The precision of the method is better, the relative standard deviation (RSD) of parallel experiment is less than 5, and the accuracy of the method is high. Conclusion the method is applied to the separation and determination of trace hydroxylamine in resagilan mesylate with high sensitivity and accurate and reliable results.
【作者單位】： 成都倍特藥業(yè)有限公司;賽默飛世爾科技(中國)有限公司;
【分類號】：R927.2

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本文編號：1538491