北京生物醫(yī)學工程

固相萃取法結合氣相色譜質譜聯用法定性定量測定一次性使用便攜式輸注泵的水溶出物

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

作者：林紅賽黃永富崔永平岳衛(wèi)華

單位：1北京市醫(yī)療器械檢驗所（北京 101111）； 2 醫(yī)療器械檢驗與安全性評價北京市重點實驗室（北京 101111）

關鍵詞：一次性使用便攜式輸注泵；固相萃取；氣相色譜-質譜；紫外吸光度；定量分析

分類號：R318.04

出版年·卷·期（頁碼）：2020·39·1（80-85）

摘要：

目的用固相萃取法(solid phase extraction，SPE)結合氣相色譜質譜聯用法(gas chromatography-mass spectrometry ,GC-MS）對一次性使用便攜式輸注泵的水溶出物進行分析，旨在分析輸注泵水溶出物的具體組成成分并分析可能導致紫外吸光度值偏高的物質。方法用紫外分光光度計對輸注泵的浸提液吸光度值進行了測定，用固相萃取技術對浸提液中的化合物進行富集，用乙酸乙酯洗脫，并用氣相色譜質譜聯用儀對浸提液組分進行定性和定量分析。采用NIST 14譜庫、離子碎片及保留時間對色譜峰進行檢索定性，并對產品中廣泛存在的物質進行定量分析。結果10個樣品中，有4個紫外吸光度超過了YY 0451-2010中0.3的限量值，氣相色譜質譜法結果顯示，溶出物定性分析共發(fā)現了17種化合物，主要是具有紫外吸收基團的酮類、酚類、酰胺類、醇類和酯類等化合物。其中環(huán)己酮、苯酚和2-乙基己醇在各產品中廣泛存在，定量分析結果顯示環(huán)己酮在D產品中高達5.2533μg/mL，苯酚在H產品中高達0.6305μg/mL，2-乙基己醇在D產品中高達0.8736μg/mL。結論采用SPE結合GC-MS法定性定量分析輸注泵水溶出物的組成，該方法準確度高、重復性好、簡便可行，可作為輸注泵水溶出物組成成分定性定量分析的方法，亦可為輸注泵浸提液紫外吸光度超標原因分析提供技術參考。

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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