心可宁胶囊中违法染色成分酸性红73检测方法的研究

目的：确认心可宁胶囊中违法染色的色素或染料成分，建立相应的染色成分分析方法。方法：采用高效液相色谱（HPLC）法对心可宁胶囊进行筛查，并采用HPLC-MS/MS二级质谱对阳性样品进行确认。质谱采用电喷雾负离子扫描（ESI^-），多反应监测模式（MRM），选择质荷比m/z 255.0→ 150.5和m/z255.0→ 241.0作为检测离子对，记录相应色谱图。在此基础上，采用HPLC法对阳性样品中的酸性红73进行含量测定。色谱条件：采用Hypersil ODS色谱柱（250 mm×4.6 mm，5μm）），以乙腈-0.05 mol·L^-1醋酸铵溶液（24：76）为流动相，流速为0.8 mL·min^-1，检测波长为509 nm。结果：采用HPLC法对213批心可宁胶囊进行筛查，并采用HPLC-MS/MS对可疑样品进行确认，有24批样品可检出酸性红73；酸性红73进样量在0.001203~1.203μg的范围内乌峰面积有良好的线性关系。24批阳性样品中酸性红73的含量范围为6.25~87.6μg·g^-1。结论：本方法准确可靠，可作为心可宁胶囊中酸性红73染色物的检测方法。  

Objective: The purpose of the research is to establish an analysis method for identification of the pigments or dyes in Xin Kening capsules. Methods: An HPLC was used as the screening method of acid red 73. The positive results of screening were confirmed by HPLC-MS/MS with ESI-ion source. The ion at m/z 255.0 → 150.5 and m/z 255.0 → 241.0 was selected for MS/MS analysis and the corresponding chromatogram was recorded. Based on those results, an HPLC method was developed for the qualification of acid red 73 in positive samples. An Hypersil ODS C₁₈ (250 mm×4.6 mm, 5 μm)column was adopted, the mixture of acetonitrile and 0.05 mol·L^-1 a mmonium acetate (24:76)was used as the mobile phase, the flow rate was 0.8 mL·min^-1, and the detection wavelength was set at 509 nm. Results: The HPLC method was used for the screening of 213 batches of Xin Kening capsules. The suspected samples were confirmed by HPLC-MS/MS. Acid red 73 was detected from 213 batches of samples. Acid red 73 had considerable linear relationship in the range of 0.001 203-1.203 μg. The content of acid red 73 in 24 batches of positive samples ranged from 6.25 to 87.6 μg·g^-1. Conclusion: This method is accurate and reliable, and can be used as the detection method for acid red 73 in Xin Kening capsules. 

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