高效液相色谱法同时测定生活用纸及纸制品中19种有机抗菌剂  

Simultaneous Determination of 19 Organic Antibacterial Agents in Tissue Paper and Paper Products by High Performance Liquid Chromatography

作　　者：綦艳 李锦清 陈满英 伍尚森 唐楚林 刘德群 QI Yan;LI Jin-qing;CHEN Man-ying;WU Shang-sen;TANG Chu-lin;LIU De-qun(Guangdong Testing Institute of Product Quality Supervision,Shunde 528300,China)

机构地区：[1]广东产品质量监督检验研究院,广东顺德528300

出　　处：《分析测试学报》2021年第7期1018-1024,共7页Journal of Instrumental Analysis

基　　金：广东省市场监督管理局科技项目(2018CZ07)。

摘　　要：建立了高效液相色谱(HPLC)同时测定生活用纸及纸制品中19种有机抗菌剂(包括7种氯苯酚类、6种季铵盐类和6种对羟基苯甲酸酯类化合物)的分析方法。样品用0.5%甲酸-甲醇溶液超声提取,经浓缩、定容后,以甲醇、乙腈和0.05%磷酸水溶液(含0.475 3 g四丁基硫酸氢铵)为流动相梯度洗脱,Welch Ultimate AQ C_(18)色谱柱(250 mm×4.6 mm,5μm)分离,采用二极管阵列检测器在191~400 nm检测。结果表明:氯苯酚类、季铵盐类和对羟基苯甲酸酯类化合物分别在0.05~20 mg/L、0.1~20 mg/L、0.02~50 mg/L质量浓度范围内呈良好线性关系(r≥0.996 0);方法检出限为0.05~0.3 mg/kg;加标回收率为74.8%~101%,相对标准偏差(RSD,n=6)为2.2%~5.6%。该方法简单、快速、准确可靠,适用于生活用纸及纸制品中19种有机抗菌剂的同时检测。In order to prevent the mildew of tissue paper and paper products,organic antibacterial agents are often used in the process of production,processing and storage.After a long-term accumulation and reaching a certain amount,the harm of the organic antibacterial agents to the environment and human body can not be ignored.However,there are few methods to detect a variety of organic antibacterial agents in tissue paper and paper products.A high performance liquid chromatographic(HPLC)method was established for the simultaneous extraction and determination of 19 organic antibacterial agents,including seven kinds of chlorophenols,six kinds of quaternary ammoniums and six kinds of p-hydroxybenzoic acid esters in tissue paper and paper products.The samples were firstly extracted twice with methanol containing 0.5%formic acid,then centrifuged at 9000 r/min for 3 min and suctioned filtration with buchner funnel to collect filtrate.The filtrate was evaporated at 45℃and condensed into about 1 mL,and then dried with nitrogen,dissolved with 2.0 mL methanol-water solution(1∶1,by volume).19 organic antibacterial agents were separated on a Welch Ultimate AQ C18 column(250 mm×4.6 mm,5μm)by gradient elution,with methanol,acetonitrile and 0.05%phosphoric acid solution(containing 0.4753 g tetrabutylammonium hydrogen sulfate)as mobile phases,then detected with photo-diode array detector(PDAD)at 191-400 nm.Results indicated that the calibration curves of chlorophenols,quaternary ammoniums and p-hydroxybenzoic acid esters showed good linear relationships in the ranges of 0.05-20 mg/L,0.1-20 mg/L and 0.02-50 mg/L,respectively,with their correlation coefficients(r)not less than 0.9960.The limits of detection(LOD,S/N≥3)for 19 organic antibacterial agents were in the range of 0.05-0.3 mg/kg.The average recoveries of this method ranged from 74.8%to 101%with relative standard deviations(RSD,n=6)of 2.2%-5.6%.The developed method was used to evaluate the 19 organic antibacterial agents in wet tissue,facial tissue and paper cups.The resu

关 键 词：高效液相色谱法 生活用纸及纸制品 有机抗菌剂 氯苯酚类化合物 季铵盐类化合物 对羟基苯甲酸酯类化合物 

分 类 号：O657.7[理学—分析化学]