摘要
目的:建立蒲黄用柠檬黄、酸性黄36染色的定性检查方法。方法:采用TLC法,对染料柠檬黄、酸性黄36进行初步检查;采用HPLC-DAD法进行验证,采用C_(18)(150 mm×4.6 mm,5μm)色谱柱,以甲醇(A)-0.2 mol·L^(-1)乙酸铵溶液(B),梯度洗脱(0~10 min,12%A,88%B;10~15 min,12%A→90%A,88%B→10%B;15~20 min,90%A→12%A,10%B→88%B;20~30 min,12%A,88%B),在428 nm波长检测柠檬黄,在422 nm波长检测酸性黄36;采用HPLC-MS法对2种色素的检出进行确证,采用乙腈-0.02 mol·L^(-1)乙酸铵(35∶65)流动相系统,ESI+扫描模式。结果:薄层色谱斑点清晰,分离度好,专属性较强。HPLC-DAD法供试样品中被检成分与对照品保留时间一致,且UV图谱一致。HPLC-MS法供试样品中相关分子离子峰及碎片特征与2种对照品一致。结论:本文所建立的方法可用于蒲黄用柠檬黄、酸性黄36染色的检查。
Objective： To establish inspection method of Typhae Pollen illegally dyed with tartrazine and metanil yellow. Methods： TLC was used to preliminary test of tartrazine and metanil yellow. Then the results were verified by HPLC-DAD method. Separation was performed on a C18 column （ 150 mm× 4.6 mm, 5 μm ） with methyl alcohol as mobile phase A and 0.2 mol · L^-1 ammonium acetate as mobile phase B using a gradient elution program （0-10 min, 12%A, 88%B; 10-15 rain, 12%A→90%A, 88%B → 10%B; 15-20 min, 90%A→ 12%A, 10%B →88%B ; 20-30 rain, 12%A, 88%B ）. The detection wavelengths were 428 nm for tartrazine and 422 nm for metanil yellow. HPLC-MS was applied to confirmation with acetonitrile-0.2 mol· L^-1 ammonium acetate （ 35 ： 65 ）as the mobile phase and positive electrospray ionization as the detection mode. Results： In TLC test, tartrazine and metanil yellow could be identified specifically by clear and well separated spots. In HPLC-DAD test, the retention times and UV spectra of the detected peaks of the test solution corresponded to those of the reference solution. In HPLC-MS test, the molecular ions and fragments of the detected peaks of the test solution corresponded to those of the reference solution. Conclusion： The method proposed in this paper could be used to test Typhae Pollen dyed with tartrazine and metanil yellow.
作者
董媛
林春燕
张赟华
耿昭
周娟
李忠琼
张雯洁
DONG Yuan LIN Chun-yan ZHANG Yun-hua GENG Zhao ZHOU Juan LI Zhong-qiong ZHANG Wen-jie(Yunnan Institute for Food and Drug Control, Kunming 650011, China Sichuan Institute for Food and Drug Control, Chengdu 610097, China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2017年第4期670-676,共7页
Chinese Journal of Pharmaceutical Analysis
