HPLC-DAD-CAD双检测器联用定量筛查清热解毒口服液中14个添加剂成分  

Quantitative screening of 14 additive components in Qingrejiedu oral liquid by HPLC-DAD-CAD

作　　者：王亚琼 钟水生 周震宇 钱岩 许奇 汪明志 张超 陈卫 薛满 WANG Ya-qiong;ZHONG Shui-sheng;ZHOU Zheng-yu;QIAN Yan;XU Qi;WANG Ming-zhi;ZHANG Chao;CHEN Wei;XUE Man(Suzhou Institute for Drug Control,Suzhou Jiangsu 215104,China)

机构地区：[1]苏州市药品检验检测研究中心,苏州215104

出　　处：《药物分析杂志》2022年第12期2136-2144,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：苏州市科技计划项目(SYS2020198)。

摘　　要：目的:建立高效液相色谱配紫外检测器及电喷雾检测器双检测器联用(HPLC-DAD-CAD)定量筛查清热解毒口服液中6个甜味剂及8个防腐剂共计14个添加剂成分。方法:口服液样品用水稀释后滤膜过滤,采用Waters Xbridge Shield RP18色谱柱(250 mm×4.6 mm,5μm),流动相为甲醇-20 mmol·L^(-1)乙酸铵水,梯度洗脱。流速:0.8 mL·min-1,柱温:35℃。采用DAD检测器:检测波长为230 nm及255 nm,同时开启全波长检测。CAD检测器:采集频率10 Hz,滤光片1 s,雾化器温度35℃。结果:14个化合物质量浓度在0.0009~0.6112 mg·mL^(-1)范围内线性良好,相关系数0.9990~1.000,平均回收率为91.2%~101.9%,RSD均<5.0%。应用该方法对200批次涉及44家企业的口服液样品进行筛查,结果防腐剂检出苯甲酸和山梨酸,甜味剂检出糖精钠和安赛蜜。苯甲酸涉及1家企业2批次样品超出药典标准限度,糖精钠涉及5家企业15批次样品,安赛蜜涉及2家企业4批次样品超出拟定限度。结论:本方法操作简便,灵敏度高,实用性好,可以同时对口服液中14个有限量的成分进行筛查。Objective:To establish a combination method of high performance liquid phase chromatography with UV detector and electrospray detector(HPLC-DAD-CAD)for quantitative screening of 14 additive components including 6 sweeteners and 8 preservatives in Qingrejiedu oral liquid.Methods:The oral solution sample was diluted with water and filtered with a membrane filter,using a Waters XBridge Shield RP18 column(250 mm×4.6 mm,5μm).The mobile phase was methanol-20 mmol·L^(-1)ammonium acetate water with gradient elution.The flow rate was 0.8 mL·min-1,and the column temperature was 35℃.Detection wavelengths ofDAD detector were 230 nm and 255 nm,and full wavelength detection was turned on at the same time.Acquisition frequency of CAD electrospray detector was 10 Hz with filter of 1 s and atomizer temperature of 35℃.Results:The concentration of 14 compounds had good linearity in the range of 0.0009-0.6112 mg·mL^(-1),the correlation coefficients were 0.9990-1.000,the average recoveries were 91.2%-101.9%,and the RSDs were all below 5.0%.The method was used to screen 200 batches of oral liquid samples involving 44 companies.As a result,benzoic acid and sorbic acid were detected,and saccharin sodium and acesulfame potassium were detected.The contents of benzoic acid in 2 batches of samples from 1 company exceeded the pharmacopoeia standard limit,saccharin sodium in 15 batches of samples from 5 companies,and acesulfame potassium in 4 batches of samples from 2 companies exceeded the proposed limit.Conclusion:The method is simple to operate,highly sensitive,and has good practicability.It can simultaneously screen 14 limited components in oral liquid.

关 键 词：双检测器联用 高效液相色谱-紫外检测器-电喷雾检测器联用(HPLC-DAD-CAD) 清热解毒口服液 防腐剂 甜味剂 定量筛查 苯甲酸 山梨酸 糖精钠 安赛蜜 

分 类 号：R917[医药卫生—药物分析学]