高效液相色谱法快速测定外用成人用品中16种局麻成分  

Rapid Determination of 16 Local Anesthetic Components in Adult Products by High Performance Liquid Chromatography

作　　者：黄艳婷[1] 庄玥 邱蕴绮[1] HUANG Yan-ting;ZHUANG Yue;QIU Yun-qi(NMPA Key Laboratory for Rapid Testing Technology of Drugs,Guangdong Institute for Drug Control,Guangzhou 510663,China)

机构地区：[1]广东省药品检验所,国家药品监督管理局药品快速检验技术重点实验室,广东广州510663

出　　处：《分析测试学报》2020年第12期1533-1537,共5页Journal of Instrumental Analysis

基　　金：2018年度广东省科技创新战略专项(2018B020207008)。

摘　　要：该文基于核壳填料色谱柱技术,建立了同时快速测定外用成人用品中16种局麻成分(普鲁卡因、丁卡因、异丁香酚甲醚、盐酸氯普鲁卡因、盐酸利多卡因、苯佐卡因、甲磺酸罗哌卡因、硫酸丁丙卡因、普鲁卡因胺、丙胺卡因、丁吡卡因、盐酸奥布卡因、丁香酚、盐酸普莫卡因、地布卡因、丁香酚甲醚)的高效液相色谱分析方法。样品经含0.1%盐酸的甲醇超声提取,采用Agilent Poroshell 120 EC-C18(50 mm×4.6 mm×2.7μm)分离,以磷酸氢二钾溶液(pH 3.0)-甲醇-乙腈为流动相进行梯度洗脱,流速1.5 mL/min,柱温35℃,二极管阵列检测器检测,检测波长为210 nm和280 nm,外标法定量。结果显示:16种局麻成分在一定质量浓度范围内线性良好,相关系数不低于0.9997。甲磺酸罗哌卡因的检出限(LOD,S/N=3)为3.1μg/g,定量下限(LOQ,S/N=10)为10.2μg/g;其余15种化合物的LOD均为1.0μg/g,LOQ为3.3μg/g;16种局麻成分在低、中、高3个加标水平下的平均回收率为93.3%~103%,相对标准偏差(RSD)为0.08%~1.2%。该方法快速、准确,适用于外用成人用品中局麻成分的快速筛查,具有广阔的应用前景。A high performance liquid chromatography(HPLC)using fused-core silica particles column was developed for the rapid determination 16 local anesthetic components,including procaine,tetracaine,methyl isoeugenol,chloroprocaine hydrochloride,lidocaine hydrochloride,benzocaine,ropivacaine mesylate,butacaine sulphate,procainamide,prilocaine,bupivacaine,benoxinate hydrochloride,eugenol,pramoxine hydrochloride,cinchocaine and methyl eugenol.The samples were ultrasonically extracted with 0.1%hydrochloride-methanol,and separated on an Agilent Poroshell 120 EC-C18(50 mm×4.6 mm×2.7μm)at 35℃by gradient elution,with dipotassium hydrogen phosphate solution(pH 3.0)-methanol-acetonitrile as mobile phase at a flow rate of 1.5 mL/min.The detection wavelengths for diode array detector were set at 210 nm and 280 nm.Quantification analysis was performed by the external standard method.Results indicated that the calibration curves for the 16 compounds showed good linearity in a certain range of mass concentration with their correlation coefficients not less than 0.9997.The limits of detection(LOD,S/N=3)and limits of quantitation(LOQ,S/N=10)for ropivacaine mesylate were 3.1μg/g and 10.2μg/g,respectively.The LODs and LOQs for other 15 compounds were 1.0μg/g and 3.3μg/g,respectively.The average recoveries at three spiked levels ranged from 93.3%to 103%,with relative standard deviations(RSD)of 0.08%-1.2%.The method was rapid and accurate,and could be used for the rapid screening of local anesthetic components in adult products,indicating its extensive application prospect.

关 键 词：快速筛查 高效液相色谱 成人用品 局麻成分 

分 类 号：O657.71[理学—分析化学]