气相色谱法定量检测注射用微球凝胶中的液体石蜡残留  

Quantitative Determination of Residual Liquid Paraffin in Microsphere Gel for Injection by Gas Chromatography

作　　者：王宝群 孙文昕 林莎莎 邹圣灿 陈醒 WANG Baoqun;SUN Wenxin;LIN Shasha;ZOU Shengcan;CHEN Xing(Qingdao Chenlan Marine Biotechnology Co.,Ltd.,Qingdao 266100,China)

机构地区：[1]青岛琛蓝海洋生物工程有限公司,山东青岛266100

出　　处：《山东化工》2024年第21期164-166,170,共4页Shandong Chemical Industry

摘　　要：液体石蜡是从石油中提取的较重烷烃的混合物,常被用作油相制备微球。但液体石蜡的体内使用可能会对人体健康产生影响。为了简单快捷地检测微球凝胶中的液体石蜡残留,对微球凝胶中的液体石蜡残留提取方法进行了优化,然后使用气相色谱-火焰离子检测器(GC-FID)检测微球凝胶中的液体石蜡残留。通过正交试验确定了凝胶中液体石蜡提取的最佳条件,使用索式提取器及石油醚在50℃条件下对微球凝胶样品进行精馏处理3 h,再用0.4 mol/L的氢氧化钾-甲醇溶液及正己烷提取凝胶中的液体石蜡,取上层液用0.22μm滤膜过滤后备用。检测选用HP-5色谱柱(30 m×0.320 mm×0.25μm),标准品配制成质量浓度0,10,30,80,90,100μg/mL。检测过程中标准品及样品分峰状态良好,标准曲线R2>0.99。方法检出限和定量限分别为2.71和8.21μg/mL。在24 h内,样品中液体石蜡测得含量结果较为稳定。样品加标回收率在85.21%~92.10%,相对标准偏差在0.94%~3.31%。该方法操作简单快捷,能够定量检测凝胶中液体石蜡残留。Liquid paraffin is a mixture of heavier alkanes extracted from petroleum.It is often used for oil phase preparation of microspheres.However,the internal use of liquid paraffin may have an impact on human health.In order to detect the residual liquid paraffin in microsphere gel simply and quickly,the extraction method was optimized,and the residual liquid paraffin in microsphere gel was detected by gas chromatography flame ion detector(GC-FID).The optimum extraction conditions of liquid paraffin in gel were determined by orthogonal test.The microsphere gel sample was rectified with a rope extractor and petroleum ether at 50℃for 3 h,and then the liquid paraffin in the gel was extracted with 0.4 mol/L potassium hydroxide methanol solution and n-hexane.Filter the upper liquid using a 0.22μm filter membrane.Detection using HP-5 chromatography column(30 m×0.320 m×0.25μm).Standard product preparation 0,10,30,80,90,100μg/mL.The standard and sample have good peak separation,and the standard curve R 2>0.99.The detection limit and quantification limit are 2.71 and 8.21μg/mL,respectively.Within 24 h,the content of liquid paraffin in the sample was relatively stable.The recovery rate of sample spiking is between 85.21%and 92.10%,and the relative standard deviation is between 0.94%and 3.31%.The method is simple and rapid,and can be used to quantitatively detect the residual liquid paraffin in gel.

关 键 词：液体石蜡 凝胶 索式提取器 气相色谱法 

分 类 号：O657.7[理学—分析化学]