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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。
OBJECTIVE To establish a method for the determination of trace hydroxylamine residues in rasagiline mesylate by spectrophotometry - online solid phase extraction - ion chromatography and provide a guarantee for the pharmacological safety of clinical drug use. Method The sample was dissolved and injected directly. Between the six-way injection valve and the chromatographic separation column, a switching valve containing a cation-enriched column, IonPac CG12A, was introduced to eliminate the rasagiline mesylate matrix on-line. After complete transfer to the IonPac CS12A column, Ion Pac CG12A was washed with acetonitrile / methanesulfonic acid solution to complete the automatic solid-phase extraction of traces of hydroxylamine residues - online analysis, amperometric detection and external standard quantification. Results The specificity and durability of the method were good. The linearity of hydroxylamine was good in 0.04 ~ 3.75μg · mL ~ (-1), the correlation coefficient (r ~ 2) was 0.999 9, the detection limit was 0.02μg · mL ~ ( -1), the limit of quantification was 0.04 μg · mL -1. The precision of the method is good, and the relative standard deviation (RSD) of the parallel test results is less than 5%. The accuracy of the method is high and the recoveries of spiked samples range from 94% to 103%. Conclusion The method is applied to the separation and determination of trace hydroxylamine in rasagiline mesylate with high sensitivity and accurate and reliable detection results.