HPLC-DAD法测定血竭饮片中添加苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ及808猩红  

Determination of sudan Ⅰ,sudan Ⅱ,sudan Ⅲ,sudan Ⅳ and 808 scarlet added in Draconis Sanguis by HPLC-DAD

作　　者：冼小敏[1] 林蔚文 陈伟康 朱寿光 XIAN Xiao-min;LIN Wei-wen;CHEN Wei-kang;ZHU Shou-guang(Dongguan Institute for Food and Drug Control,Dongguan 523808,China)

机构地区：[1]东莞市食品药品检验所,东莞523808

出　　处：《药物分析杂志》2020年第5期865-872,共8页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立HPLC-DAD对血竭饮片中非法添加苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ及808猩红的定性和同时定量方法。方法:采用Kromasil100-5 C18色谱柱(250 mm×4.6 mm,5μm),以乙腈-水(90∶10)为流动相,流速1.0 mL·min^-1,检测波长478 nm(苏丹红Ⅰ)和520 nm(苏丹红Ⅱ、Ⅲ、Ⅳ、808猩红)。结果:5个色素分离度良好;苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ、808猩红质量浓度分别在0.5128~20.5128μg·mL^-1(r=1.000)、0.4965~19.8594μg·mL^-1(r=1.000)、0.4951~19.8058μg·mL^-1(r=1.000)、0.4771~19.0820μg·mL^-1(r=1.000)和0.5064~20.2554μg·mL^-1(r=1.000)内线性关系良好;精密度RSD小于0.30%;3个加样浓度的平均回收率(n=6)为98.9%~106.6%;重复性RSD为0.51%~1.8%;5个成分在48 h内保持稳定,RSD小于3.0%。20批样品中,3批为阳性样品,其中1批掺入苏丹红Ⅳ,2批掺入808猩红,含量分别为3.0、3.8、2.0 mg·g^-1。结论:该方法简便准确,可用于血竭饮片中非法添加苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ、808猩红5个合成色素的定性鉴别和含量测定。Objective:To establish an HPLC-DAD method for simultaneous qualitative and quantitative analysis of sudanⅠ,sudanⅡ,sudanⅢ,sudanⅣand 808 scarlet illegally added in Draconis Sanguis.Methods:The separation was performed on a Kromasil 100-5 C18(250 mm×4.6 mm,5μm)column and the mobile phase consisted of acetonitrile-water(90∶10)at a flow rate of 1.0 mL·min^-1.The detection wavelength was 478 nm(sudanⅠ)and 520 nm(sudanⅡ,sudanⅢ,sudanⅣand 808 scarlet).Results:The five synthetic pigments were well separated.The linear ranges of sudanⅠ,sudanⅡ,sudanⅢ,sudanⅣ,808 scarlet were 0.5128-20.5128μg·m L^-1(r=1.000),0.4965-19.8594μg·m L^-1(r=1.000),0.4951-19.8058μg·m L^-1(r=1.000),0.4771-19.0820μg·mL^-1(r=1.000)and 0.5064-20.2554μg·mL^-1(r=1.000).The results of the precision tests were satisfactory with relative standard deviations(RSDs)all below 0.30%.The average spike recoveries(n=6)at three concentration levels were 98.9%-106.6%and RSDs were 0.51%-1.8%.The results of the stability tests were satisfactory and the five synthetic pigments remained stable in 48 hours with all RSDs below 3.0%.Among 20 batches of samples,3 batches were positive samples,including 1 batch mixed with SudanⅣand 2 batches mixed with 808 scarlet,with the content of 3.0,3.8 and 2.0 mg·g^-1,respectively.Conclusion:The method is simple and accurate,which can be used for qualitative and quantitative determination of sudanⅠ,sudanⅡ,sudanⅢ,sudanⅣand 808 scarle illegally added in Draconis Sanguis.

关 键 词：血竭 苏丹红Ⅰ 苏丹红Ⅱ 苏丹红Ⅲ 苏丹红Ⅳ 808猩红 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]