摘要
目的：建立气相色谱-串联质谱（GC—MS／MS）测定输注类医疗器械产品中粘合剂环己酮分析方法。方法：采用HP-5MS石英毛细管柱（30m×0．25mm×0．25μm），全扫描总离子图（TIC0）定性，选择离子检测（SIM）定量。样品经乙醇提取，室温下利用蠕动泵对输液器中的环己酮进行提取，提取液经气相色谱一串联质谱分析。结果：环己酮浓度在1．0～40μg·mL^-1。范围内呈良好线性，相关系数为0．9995，检出限（S／N=3）为0．037μg·mL^-1，定量下限（SIN=10）为0．37μg·mL^-1，平均加标回收率（n=3）为96％～99％，RSD为1．5％～1．7％。结论：该方法简便快速，定性定量准确，灵敏度高，可作为一次性使用输液器环己酮残留量控制的方法之一。
Objective：To established an effective GC - MS/MS method for the content determination of residual cyclohexanone in disposable infusion sets. Methods： The HP - 5 MS capillary column （ 30 m × 0.25 mm × 0.25 μm） was adopted, and qualitative and quantitative analysis was performed by selective ion monitoring（SIM） and total ion chromatography （TIC） of full scan. Cyclohexanone in disposable infusion sets was extracted with circular pump, using ethyl alcohol as the extraction solvent, and then the extract was analyzed by gas chromatography - tandem mass spectrometry. Results： Cyclohexanone showed good linearity in the range of 1.0 -40 μg · mL^-1. The correla- tion coefficient was 0. 9995. The detection limit （ LOQ, SIN = 3 ） of cyclohexanone was 0. 037μg · mL^-1 and limit of quantitation（S/N = 10）was 0. 37μg · mL^-1. The spiked average recovery（n =3）ranged from 96% to 99%. The rela- tive standard deviation（RSD） of the method ranged from 1.5% to 1.7%. Conclusion： The method is simple, rapid, sensitive and accurate, and may serve as a mass control method for residual eyclohexanone in disposable infusion sets.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2014年第4期711-713,共3页
Chinese Journal of Pharmaceutical Analysis
基金
浙江省科技厅计划项目(2012F30002)
项目名称:环己酮为粘合剂的输液(血)器安全性评价研究
关键词
输液器
气相色谱-质谱法
环己酮
乙醇
粘合剂残留量控制
infusion set
gas chromatography - tandem mass spectrometry
cyclohexanone
ethyl alcohol
adhesive residue control
