固相萃取结合HPLC法同时测定头孢克洛干混悬剂中6种合成色素含量  

Simultaneous determination of six synthetic pigments in cefaclor for suspension by HPLC combined with solid phase extraction

作　　者：郝伟 徐可 朱娜 刘云 刘剑[2] HAO Wei;XU Ke;ZHU Na;LIU Yun;LIU Jian(Shijiazhuang Institute for Food and Drug Control,Shijiazhuang 050011,China;Beijing Institute of Nutritional Resources Co.,Ltd.,Beijing 100069,China)

机构地区：[1]石家庄市食品药品检验中心,石家庄050011 [2]北京市营养源研究所有限公司,北京100069

出　　处：《中国药品标准》2022年第3期334-340,共7页Drug Standards of China

摘　　要：目的:建立固相萃取结合HPLC(高效液相色谱)法同时测定头孢克洛干混悬剂中6种合成色素含量。方法:使用固相萃取柱Welchrom®PA(1g∶6 mL)对6种合成色素进行萃取富集,再用HPLC法测定其含量。该药物富集提取液的分析采用色谱柱Waters XBridge®Shield RP_(18)(4.6 mm×250 mm,5μm);流动相为甲醇(A)-0.02 mol·mL^(-1)醋酸铵溶液(B),梯度洗脱;流速1.0 mL·min^(-1);合成色素的检测波长为各自的最大吸收波长(柠檬黄428 nm,日落黄483 nm,胭脂红509 nm,苋菜红521 nm,赤藓红529 nm,靛蓝608 nm);柱温30℃。结果:6种合成色素均在1.0~25.0μg·mL^(-1)范围内呈良好的线性关系(r≥0.9999),平均加标回收率均大于99.0%,样品测定重复性RSD小于1.0%。结论:该方法操作简便,重复性好,专属性强,可用于头孢克洛干混悬剂的质量控制。Objective:To establish an HPLC method combined with solid phase extraction for simultaneous determination of six synthetic pigments in cefaclor for suspension.Methods:Six synthetic pigments were extracted and enriched with solid phase extraction column Welchrom®PA(1 g∶6 mL)and determined by HPLC.The test was performed in Waters XBridge®Shield RP_(18) column(4.6 mm×250 mm,5μm)under the gradient elution of methanol(mobile phase A)-0.02 mol·mL^(-1) ammonium acetate solution(mobile phase B).The flow rate was 1.0 mL·min^(-1),and the column temperature was 30℃.The detection wavelengths of synthetic pigments were respectively the maximum absorption wavelengths(tartrazine 428 nm,sunset yellow 483 nm,cochineal red 509 nm,amaranth 521 nm,erythrosine 529 nm,indigo blue 608 nm).Results:The linear ranges of six pigments fell into 1.0-25.0μg·mL^(-1) with r≥0.9999.The average spiked recoveries were more than 99.0%,and the RSDs of repeatability were less than 1.0%.Conclusion:The established method was simple,repeatable and specific.It can be used for quality control of cefaclor for suspension.

关 键 词：头孢克洛干混悬剂 柠檬黄 日落黄 胭脂红 苋菜红 赤藓红 靛蓝 固相萃取 高效液相色谱 

分 类 号：R921.2[医药卫生—药学]