高效液相色谱法同时测定医用敷料类医疗器械产品中17种对羟基苯甲酸酯类化合物的含量  

Simultaneous Determination of 17 Hydroxybenzoate Compounds in Medical Dressing Category Medical Device Products by High Performance Liquid Chromatography

作　　者：周羽晗 袁榕穗 段玉林 边贺东 张玉贞 韦家荣 陆兰娟 蒋受军 ZHOU Yuhan;YUAN Rongsui;DUAN Yulin;BIAN Hedong;ZHANG Yuzhen;WEI Jiarong;LU Lanjuan;JIANG Shoujun(School of Chemistry and Chemical Engineering,Guangxi University for Nationalities,Nanning 530006,China;Guangxi Zhuang Autonomous Region Food and Drug Evaluation and Inspection Center,Nanning 530029,China;Guangxi Minsheng Sino Assessment Group Co.,Ltd.,Nanning 530007,China)

机构地区：[1]广西民族大学化学化工学院,南宁530006 [2]广西壮族自治区食品药品审评查验中心,南宁530029 [3]广西民生中检联检测有限公司,南宁530007

出　　处：《理化检验（化学分册）》2024年第12期1252-1256,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：广西药品监督管理局2024年药品安全科研项目(桂药监办函[2024]177号);广西科技基地和人才专项(桂科AD20238043)。

摘　　要：在医用敷料类医疗器械产品(样品)中加入体积比8∶2的甲醇-乙腈混合溶液提取后,涡旋混匀,超声提取,离心分离,上清液过0.22μm滤膜,滤液进入高效液相色谱仪,对羟基苯甲酸酯类化合物(PBs)在ShimNex CS C_(18)色谱柱上用不同体积比的乙腈-0.12%(体积分数)磷酸溶液的混合溶液梯度洗脱分离,外标法定量。结果显示,17种PBs的质量浓度在1~50 mg·L^(-1)内和峰面积呈线性关系,检出限(3S/N)为5~18 mg·kg^(-1);按照标准加入法进行回收试验,回收率为97.6%~108%,测定值的相对标准偏差(n=6)为0.30%~4.4%;利用该方法筛查10批不同基质的实际样品,PBs检出率为40%,检出对羟基苯甲酸甲酯的样品有1批、对羟基苯甲酸乙酯和对羟基苯甲酸丙酯的样品有3批。After adding the mixed solution of methanol and acetonitrile at volume ratio of 8∶2 into samples of medical dressing category medical device products,vortex mixing,ultrasonic extraction,and centrifugal separation were performed.The supernatant was passed through a 0.22μm filter membrane,and the filtrate was introduced into the high performance liquid chromatograph.Hydroxybenzoate compounds(PBs)were separated by gradient elution with mixed solutions of acetonitrile and 0.12%(volume fraction)phosphoric acid solution at different volume ratios on the ShimNex CS C_(18) column,and quantified by the external standard method.It was shown that linear relationships between values of mass concentration and peak area of 17 PBs were kept in the range of 1-50 mg·L^(-1),with detection limits(3S/N)in the range of 5-18 mg·kg^(-1).Test for recovery was made according to the standard addition method,giving recoveries in the range of 97.6%-108%,and RSDs(n=6)of the determined values ranged from 0.30%to 4.4%.This method was used to screen 10 batches of actual samples with different matrices,and the detection rate of PBs was 40%.Methyl p-hydroxybenzoate was detected in 1 batch of samples,and ethyl p-hydroxybenzoate and propyl p-hydroxybenzoate were detected in 3 batches of samples.

关 键 词：医用敷料类医疗器械产品 对羟基苯甲酸酯类化合物 高效液相色谱法 测定 

分 类 号：O657.7[理学—分析化学]