摘要
目前标准方法检测苯扎氯铵时仅用了一个平均相对分子质量洁尔灭来表示两种或几种混合物,无法区别苯扎氯铵的几种同系物,为了测定苯扎氯铵同系物的含量,进行了题示研究。取消毒产品1.0000 g,用水稀释并定容至10 mL,超声提取5 min,静置,过0.45μm聚砜醚水相滤膜,滤液中苯扎氯铵3种同系物十二烷基二甲基苄基氯化铵、十四烷基二甲基苄基氯化铵、十六烷基二甲基苄基氯化铵在Agilent XDB-C_(18)色谱柱(250 mm×4.6 mm,5μm)上分离,以体积比70:30的乙腈-含0.1%(体积分数)三乙胺的0.5 g·L^(-1)乙酸铵缓冲溶液(pH 5.0)为流动相进行等度洗脱,采用二极管阵列检测器在262 nm处检测。结果表明,扫尾剂三乙胺的体积分数从1%降低到0.1%,避免了扫尾剂三乙胺对色谱柱的可能损害,解决了出现鬼峰的问题。苯扎氯铵3种同系物的质量浓度在10~500 mg·L^(-1)内与对应的峰面积呈线性关系,检出限(3S/N)分别为1.1,1.2,1.5 mg·L^(-1)。按照标准加入法进行回收试验,回收率为98.8%~105%,测定值的相对标准偏差(n=8)均小于2.0%。方法用于实际消毒产品的分析,检出量为0.027%~44.60%,从微量到常量均有涉及。
At present,the standard method for detecting benzalkonium chloride only uses an average relative molecular weight(geramine)to represent two or several mixtures,which cannot distinguish several homologues of benzalkonium chloride.In order to determine benzalkonium chloride homologues,the study mentioned by the title was proposed.1.0000 g of disinfection product was taken,diluted with water to 10 mL,extracted for 5 min by ultrasound and settled.The solution was passed through 0.45μm polysulfone ether aqueous phase filter membrane.Three homologues of benzalkonium chloride,dodecyl dimethyl benzyl ammonium chloride,tetradecyl dimethyl benzyl ammonium chloride,and hexadecyl dimethyl benzyl ammonium chloride,in the filtrate were separated on Agilent XDB-C_(18) column(250 mm×4.6 mm,5μm),eluted isocratically with a miture of acetonitrile and 0.5 g·L^(-1) ammonium acetate buffer solution(pH 5.0)containing 0.1%(volume fraction)triethylamine at volume ratio of 70\:30,and detected at 262 nm by a diode array detector.As shown by the results,the volume fraction of the sweeping agent triethylamine was reduced from 1%to 0.1%,avoiding the possible damage of the sweeping agent triethylamine to the chromatographic column and solving the problem of ghost peaks.Linear relationships between values of the corresponding peak area and mass concentration of three homologues of benzalkonium chloride were found in the range of 10-500 mg·L^(-1),with detection limits(3S/N)of 1.1,1.2,1.5 mg·L^(-1),respectively.Test for recovery was made by the standard addition method,giving the results in the range of 98.8%-105%,with RSDs(n=8)of the determined values less than 2.0%.This method was used for the analysis of actual disinfection products,with detection amounts in the range of 0.027%-44.60%,involving both trace and constant amounts.
作者
陈松辉
钱辉
李兴根
汶海花
朱磊
王爱霞
CHEN Songhui;QIAN Hui;LI Xinggen;WEN Haihua;ZHU Lei;WANG Aixia(China National Fine Chemicals Quality Inspection and Testing Center,Taizhou Institute of Product Quality Supervision and Inspection,Taizhou 225300,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2024年第3期294-299,共6页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
关键词
反相液相色谱-二极管阵列法
消毒产品
苯扎氯铵
同系物
reversed phase liquid chromatography with diode array detection
disinfection product
benzalkonium chloride
homologues
