北京生物医学工程

固相萃取法结合气相色谱质谱联用法定性定量测定一次性使用便携式输注泵的水溶出物

Qualitative and quantitative determination of water extracts from portable infusion devices for single use by solid phase extractionand gas chromatography-mass spectrometry

作者：林红赛黄永富崔永平岳卫华

单位：1北京市医疗器械检验所（北京 101111）； 2 医疗器械检验与安全性评价北京市重点实验室（北京 101111）

关键词：一次性使用便携式输注泵；固相萃取；气相色谱-质谱；紫外吸光度；定量分析

分类号：R318.04

出版年·卷·期（页码）：2020·39·1（80-85）

摘要：

目的用固相萃取法(solid phase extraction，SPE)结合气相色谱质谱联用法(gas chromatography-mass spectrometry ,GC-MS）对一次性使用便携式输注泵的水溶出物进行分析，旨在分析输注泵水溶出物的具体组成成分并分析可能导致紫外吸光度值偏高的物质。方法用紫外分光光度计对输注泵的浸提液吸光度值进行了测定，用固相萃取技术对浸提液中的化合物进行富集，用乙酸乙酯洗脱，并用气相色谱质谱联用仪对浸提液组分进行定性和定量分析。采用NIST 14谱库、离子碎片及保留时间对色谱峰进行检索定性，并对产品中广泛存在的物质进行定量分析。结果10个样品中，有4个紫外吸光度超过了YY 0451-2010中0.3的限量值，气相色谱质谱法结果显示，溶出物定性分析共发现了17种化合物，主要是具有紫外吸收基团的酮类、酚类、酰胺类、醇类和酯类等化合物。其中环己酮、苯酚和2-乙基己醇在各产品中广泛存在，定量分析结果显示环己酮在D产品中高达5.2533μg/mL，苯酚在H产品中高达0.6305μg/mL，2-乙基己醇在D产品中高达0.8736μg/mL。结论采用SPE结合GC-MS法定性定量分析输注泵水溶出物的组成，该方法准确度高、重复性好、简便可行，可作为输注泵水溶出物组成成分定性定量分析的方法，亦可为输注泵浸提液紫外吸光度超标原因分析提供技术参考。

Objective The water extracts from portable infusion devices for single-use are determined by gas chromatography-mass spectrometry with a solid phase extraction procedure. The purpose of this study is to analyze the components of water extracts and the substances that may cause high ultraviolet absorbance. Methods Ultraviolet spectrophotometer was used to determine the absorbance value of water extract. Solid phase extraction technology was used to enrich the compounds in the extract and ethyl acetate was used to elute them. The components of water extracts were qualitatively and quantitatively analyzed by gas chromatography-mass spectrometry. Chromatographic peaks were retrieved and analyzed using the NIST 14 spectral library, as well as its ion fragments and retention time. Quantitative analysis of substances widely existing in products was also carried out. Results Among the 10 samples, ultraviolet absorbance of 4 samples exceeded the limit of 0.3 in YY 0451-2010. Gas chromatography-mass spectrometry showed that 17 potential compounds were found in the qualitative analysis such as ketones, phenols, amides, alcohols and esters. Cyclohexanone, phenol and 2-ethyl hexanol were widely found in various products. Quantitative analysis showed that cyclohexanone was 5.2533μg/mL in D products, phenol was 0.6305μg/mL in H products and 2-ethylhexanol was 0.8736μg/mL in D products. Conclusions The SPE combined with GC-MS is used to quantitatively analyze the composition of water extracts. The method has high accuracy, good repeatability, simple and feasible, and can be used as a qualitative and quantitative analysis method for the composition of water extracts. Also it can provide technical reference for the analysis of the cause of the high ultraviolet absorbance of water extracts

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