高效液相色谱-蒸发光散射检测法同时测定口腔护理产品中10种季铵盐类杀菌剂  

Simultaneous determination of 10 quaternary ammonium salt bactericides in oral care products by high performance liquid chromatography⁃evaporative light⁃scattering detection

作　　者：汤娟 丁友超 费晓庆 吴斌 钱志娟 陈山丹 李柏 TANG Juan;DING Youchao;FEI Xiaoqing;WU Bin;QIAN Zhijuan;CHEN Shandan;LI Bai(Industrial Products Testing Center,Nanjing Customs,Nanjing 210019,China;Animal,Plant and Food Inspection Center,Nanjing Customs,Nanjing 210019,China;Light Industrial Products and Children’s Products Inspection Center,Nanjing Customs,Yangzhou 225009,China;Nanjing Jinjian Inspection Co.,Ltd.,Nanjing 210019,China)

机构地区：[1]南京海关工业产品检测中心,江苏南京210019 [2]南京海关动植物与食品检测中心,江苏南京210019 [3]南京海关轻工产品与儿童用品检测中心,江苏扬州225009 [4]南京金检检验有限公司,江苏南京210019

出　　处：《色谱》2024年第8期783-791,共9页Chinese Journal of Chromatography

基　　金：海关总署科研项目(2022HK028)。

摘　　要：建立了同时测定口腔护理产品中10种季铵盐类杀菌剂的高效液相色谱-蒸发光散射(HPLC-ELSD)检测方法。在采用无水硫酸钠脱水后的膏体样品和粉末样品中加入乙醇,常温超声提取;液体样品用乙醇稀释。采用Acclaim Surfactant色谱柱(150 mm×4.6 mm,5μm)进行分离,以50 mmol/L乙酸铵缓冲溶液(pH=5.5)和乙腈为流动相进行梯度洗脱,外标法定量。结果表明,10种目标化合物在25 min内完成色谱分离,检出限(信噪比(S/N)=3)和定量限(S/N=10)分别为1.42~3.31 mg/L和4.25~9.94 mg/L。十八烷基二甲基苄基氯化铵和二十二烷基三甲基氯化铵在10~200 mg/L范围内线性关系良好,其余目标物在5~100 mg/L范围内线性关系良好,10种季铵盐类杀菌剂的相关系数(R^(2))均不小于0.9992。以阴性样品牙膏(膏体)、漱口水(液体)和洁牙粉(粉末)为样品基质,在不同添加水平下,10种季铵盐类杀菌剂的平均回收率为87.9%~103.1%,相对标准偏差(RSD,n=6)均不大于5.5%。本方法在液相色谱分离时采用表面活性剂色谱柱,目标化合物均获得较好保留,同时采用蒸发光散射检测器,部分无紫外吸收的目标化合物也能得到较高响应。通过添加适量无水硫酸钠去除膏体样品中的水分,有利于样品前处理和保护色谱柱。本方法精密度好,准确度高,适用于各种口腔护理产品中季铵盐类杀菌剂的测定,为口腔护理产品的质量安全监控提供了参考。采用本方法对109个常用口腔护理产品进行测定,十六烷基二甲基苄基氯化铵和十八烷基二甲基苄基氯化铵的检出率较高,1个牙膏样品中十八烷基二甲基苄基氯化铵的含量超出法规要求,测定值为1511 mg/kg。Quaternary ammonium salt bactericides are broad-spectrum bactericides often used in oral care products because of their high antibacterial efficacy,strong penetration,and low toxicity.However,the excessive use of quaternary ammonium salt bactericides may cause contact dermatitis,scalding poisoning,and even death.Existing methods to determine quaternary ammonium salt bactericides are unable to meet current requirements owing to the lack of determination components.Therefore,establishing a simple and accurate method for the simultaneous detection of more quaternary ammonium salt bactericides is necessary.In this study,a method that couples sample pretreatment with high performance liquid chro⁃matography⁃evaporative light⁃scattering detection(HPLC-ELSD)was developed for the simulta⁃neous determination of quaternary ammonium salt bactericides in oral care products,including dodecyltrimethylammonium chloride,dodecyldimethylbenzylammonium chloride,benzethoni⁃um chloride,tetradecyl trimethyl ammonium chloride,tetradecyldimethylbenzylammonium chloride,N⁃hexadecyltrimethylammonium chloride,benzyldimethylhexadecylammonium chlo⁃ride,trimethylstearylammonium chloride,stearyldimethylbenzylammonium chloride,and doco⁃syltrimethylammonium chloride.Some of these bactericides do not absorb ultraviolet light,so a universal evaporative light⁃scattering detector was used owing to testing cost and stability con⁃cerns.The paste samples contained thickening agents,which are highly soluble in water but in⁃soluble in organic solvents;these agents can seriously affect the results of sample pretreatment and damage the chromatographic column.Hence,sample dehydration was necessary.In this study,four dehydration methods were compared.Anhydrous sodium sulfate(Na_(2)SO_(4))was se⁃lected,and the amount of Na_(2)SO_(4)was optimized.Based on the solubility of the 10 target com⁃pounds and extraction efficiency,three extraction solvents were compared,and ethanol was selected.Ultrasonic extraction was the primary extraction p

关 键 词：高效液相色谱 蒸发光散射检测 季铵盐 杀菌剂 口腔护理产品 

分 类 号：O658[理学—分析化学]