LC-MS/MS同时测定朱砂中掺假染料猩红808和玫瑰红B的含量

Simultaneous Determination of Red Adulterated Dye Scarlet 808 and Rhodamine B in Cinnabar by LC-MS/MS

关键词:  LC-MS/MS  朱砂  猩红808  玫瑰红B

Key words:  LC/MS/MS  cinnabar  scarlet 808  rhodamine B

摘要:

目的 建立液相色谱-串联质谱(LC-MS/MS)法同时测定朱砂中的掺假染料猩红808和玫瑰红B的含量。方法 采用Agilent ZORBAX SB-C₁₈(2.1 mm×50 mm，1.8 μm)色谱柱，流动相为乙腈-0.1%甲酸溶液，流速为0.3 mL·min^-1，柱温为30 ℃，离子化方式为ESI，检测模式为MRM，选择离子对：①猩红808 m/z 368.1→275.1，m/z 368.1→219.1，m/z 368.1→77.1；②玫瑰红B m/z 443.2→399.2，m/z 443.2→355.0。结果 该方法猩红808和玫瑰红B的线性范围为10~200 ng·mL^-1和9.69~193.8 ng·mL^-1；检测限分别为2 ng·mL^-1和1.9 ng·mL^-1；回收率(n=6)分别为97.86%和97.34%，RSD为0.70%和0.73%；精密度、稳定性和重复性的RSD均<4%。结论 该方法提取简单，测定方法定量准确，确证性极高、灵敏高，适用于朱砂中红色染料猩红808和玫瑰红B的含量测定，还可为其他红色中药的安全检测提供了借鉴依据。

Abstract:

OBJECTIVE Establish a method for simultaneous determination of adulteration cinnabar dye scarlet 808 and Rhodamine B By LC-MS/MS. METHODS Using Agilent ZORBAX SB-C₁₈(2.1 mm×50 mm, 1.8 μm) column, mobile phase of acetonitrile-0.1% formic acid, the flow rate was 0.3 mL·min^-1, column temperature was 30 ℃, ethanol as an extraction solvent, Ionization mode was ESI, detection mode was MRM. Selected ion pair: ①Scarlet 808 m/z 368.1→275.1, m/z 368.1→219.1, m/z 368.1→77.1; ②Rhodamine B m/z 443.2→399.2, m/z 443.2→355.0. RESULTS the linear range of A and B was 10~200 ng·mL^-1 and 9.69~193.8 ng·mL^-1 in this method; detection limit was 2 ng·mL^-1 and 1.9 ng·mL^-1; recoveries were 97.86% and 97.34%, RSD was 0.70% and 0.73%; precision, stability and repeatability of RSD were less than 4%. CONCLUSION The method of extraction is simple, determination is accurate, confirmatory high, high sensitivity, determination red dye Scarlet 808 and Rhodamine B are applicable to cinnabar, and also provide a reference basis for the safety testing of other Chinese medicine with red color.