气相色谱-质谱联用法测定一次性使用输液器中环己酮的残留量

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（30 m×0.25 mm×0.25 μm），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-串联质谱分析。 结果： 环己酮浓度在1.0～40 μg·mL^-1范围内呈良好线性，相关系数为0.9995，检出限（S/N=3）为0.037 μg·mL^-1，定量下限（S/N=10）为0.37 μg·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-5MS 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 correlation coefficient was 0.9995.The detection limit(LOQ,S/N=3)of cyclohexanone was 0.037 μg·mL^-1 and limit of quantitation(S/N=10)was 0.37 μg·mL^-1.The spiked average recovery(n=3)ranged from 96% to 99%.The relative 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 cyclohexanone in disposable infusion sets.

[1] ZHANG En-juan(张恩娟),LIU Tong-hua(刘同华),JIANG Min(江敏),et al.Infusion plastic products of drug absorption(输液用塑料制品对药物的吸附)[J].China Pharm(中国药房),2003,14(11):693
[2] DONG Zhen-hai(董振海),XU Hong-xia(许红霞),DONG Hua-jun(董华军).Polyvinyl chloride(PVC)infusion and glass products for the adsorption effect of drugs(聚氯乙烯输液器及玻璃制品对药物的吸附作用)[J].Chin J Med(中国医刊),2004,39(4):48
[3] WANG Yan-ming(王焰民).Research of residual cyclohexanone indisposable infusion set(对一次性使用输液(血)器环己酮残留量的调查).China Pharm(中国药房),1992,3(6):45
[4] JIANG Wen-qiang(蒋文强),QIN Dong-li(秦冬立),WANG Xin(王昕).Studying on cyclohexanone for infusion(transion)set(输液器中的环己酮的研究)[J].Shandong J Biomed Eng(山东生物医学工程),1997,16(3):50
[5] JIANG Wen-qiang(蒋文强),LV Xia(吕霞).Determination of residual cyclohexanone in disposable infusion set by UV(一次性使用输液器水浸液中环己酮的分光光度法测定)[J].Chin J Pharm Anal(药物分析杂志),1998,18(3):195
[6] DONG Jin(董荩),DING Jian(丁建).GC determination of residual cyclohexanone in disposable infusion set(气相色谱法测定一次性使用输液器中环己酮的残留量)[J].Chin J Pharm Anal(药物分析杂志),2009,29(6):1022
[7] GB 8368-2005,Infusion Sets for Single Use,Gravity Feed(一次性使用输液器重力输液式)[S].2005