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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,1.8μm)色谱柱,流动相为乙腈-0.1%甲酸溶液,流速为0.3 m L·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/z368.1→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·m L?1和9.69~193.8 ng·m L?1;检测限分别为2 ng·m L?1和1.9 ng·m L?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。
Objective To establish a liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for the simultaneous determination of adulterated dyes Scarlet 808 and Rose B in cinnabar. Methods The mobile phase consisted of acetonitrile-0.1% formic acid solution at a flow rate of 0.3 m L · min -1 with a ZORBAX SB-C18 column (2.1 mm × 50 mm, 1.8 μm). The column temperature was 30 ℃ and the ionization mode was ESI, detection mode MRM, Selected ion pair: 1 Scarlet 808 m / z 368.1 → 275.1, m / z 368.1 → 219.1, m / z 368.1 → 77.1; 2 Rose B m / z 443.2 → 399.2, m / z 443.2 → 355.0. Results The calibration curves of Scarlet 808 and Rose B were linear in the range of 10-200 ng · m L -1 and 9.69-193.8 ng · m L -1, with the detection limits of 2 ng · m L -1 and 1.9 ng · m L, respectively 1; the recoveries (n = 6) were 97.86% and 97.34%, respectively. The RSDs were 0.70% and 0.73%, respectively. The RSDs of precision, stability and repeatability were all less than 4%. Conclusion The method is simple, accurate, accurate and reliable. It is suitable for the determination of red dye Scarlet 808 and Rose B in cinnabar. It can also provide references for the safety testing of other red Chinese medicines.