目的 建立冠脉宁片中化工染料检查及血竭素高氯酸盐含量测定方法。方法 采用高效液相色谱-串联质谱联用法(HPLC-MS/MS)对冠脉宁片中血竭药材可能存在的化工染料进行检查,并采用高效液相色谱法对其中的血竭素含量进行测定。化工染料检查使用色谱柱为:Agilent Zorbax-SB C₁₈(4.6 mm×250 mm,5 μm),流动相为0.02 mol·L^-1乙酸铵和乙腈的混合溶液,梯度洗脱,520 nm检测;质谱采用ESI⁺扫描,二级离子扫描方式。血竭素含量测定使用的色谱柱为Phenomenex Luna C₁₈(4.6 mm×250 mm,5 μm)柱,流动相为乙腈-0.05 mol·L^-1磷酸二氢钠溶液(37∶63),检测波长440 nm。结果 56批次样品中共有7批样品可检出苏丹红Ⅰ、Ⅳ以及808猩红等化工染料。血竭素高氯酸盐在0.408～816.6 μg·mL^-1内有良好的线性关系,回归方程为y=1.746 1×10⁷ρ+2 419.9,r=1.000 0;平均回收率为98.37% (RSD为1.2%,n=6)。56批次样品中血竭素含量在0.01~0.25 mg·片^-1内。结论 所建立的方法简便,准确,快速,可用于冠脉宁片中血竭药材的质量控制。

OBJECTIVE To establish METHODS for the test of chemical dyes and quantitative determination of dracorhodin perchlorate in Guanmaining tablets. METHODS HPLC-UV-MS/MS was used for the test of chemical dyes in Guanmaining tablets, and the concentration of dracorhodin perchlorate was determined by HPLC. In the test of chemical dyes, Agilent Zorbax-SB C₁₈(4.6 mm×250 mm,5 μm) was used as stationary phase, the mixture of 0.02 mol·L^-1 ammonium acetate and acetonitrile was used as mobile phase in gradient elution mode, and the UV-Vis detection wavelength was set at 520 nm. ESI⁺ was used as ion source, and the MS/MS spectra of the analytes were recorded to confirm the positive results. In the quantitative analysis of dracorhodin perchlorate, Phenomenex Luna C₁₈(4.6 mm×250 mm,5 μm) was used as stationary phase, the mixture of acetonitrile and 0.05 mol·L^-1 sodium dihydrogen phosphate solution (37∶63) was used as mobile phase, and the detection wavelength was set at 440 nm. RESULTS Among 56 batches of Guanmaining tablets, 7 batches showed positive RESULTS of sudan Ⅰ, sudan Ⅳ, and/or 808 scarlet. A good linear relationship was obtained in the range of 0.408 0-816.6 μg·mL^-1 for dracorhodin perchlorate, with the linear regression equation of y=1.746 1×10⁷ρ+2 419.9(r=1.000 0); the average recovery was 98.37%(RSD=1.2%, n=6). The content of dracorhodin perchlorate in Guanmaining tablets ranged from 0.01 to 0.25 mg·tablet^-1. CONCLUSION The method is simple, accurate and rapid,and can be used for the quality control of Guanmaining tablets.