在线固相萃取-离子色谱法测定甲磺酸雷沙吉兰中残留羟胺含量

发布时间：2018-02-26 14:55

本文关键词： 离子色谱甲磺酸雷沙吉兰羟胺　出处：《中国药学杂志》2017年20期 　论文类型：期刊论文

【摘要】：目的建立谱睿-在线固相萃取-离子色谱法测定甲磺酸雷沙吉兰药品中痕量羟胺残留含量的分析方法,为临床用药的药学安全性提供保障。方法样品经溶解后直接进样,在六通进样阀和色谱分离柱之间,引入含阳离子富集柱——IonPac CG12A的切换阀,在线消除甲磺酸雷沙吉兰样品基体,待羟胺完全转移至IonPac CS12A柱上后,以乙腈/甲基磺酸溶液清洗Ion Pac CG12A,完成了痕量羟胺残留含量的自动固相萃取-在线分析,安培检测,外标法定量。结果方法专属性、耐用性良好,羟胺在0.04~3.75μg·mL~(-1)内具有良好的线性,相关系数(r~2)为0.999 9,其检出限为0.02μg·mL~(-1),定量限为0.04μg·mL~(-1)。方法精密度较好,平行实验检测结果相对标准偏差(RSD)小于5%;方法准确度较高,加标回收率介于94%~103%之间。结论本方法应用于甲磺酸雷沙吉兰中痕量羟胺的分离测定,灵敏度高,检测结果准确可靠。
[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.
【作者单位】：成都倍特药业有限公司;赛默飞世尔科技(中国)有限公司;
【分类号】：R927.2

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