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目的:建立同时测定注射用辛芍(冻干粉针)中没食子酸、氧化芍药苷、芍药内酯苷、芍药苷、野黄芩苷、灯盏甲素和苯甲酰芍药苷含量的UPLC-MS/MS方法。方法:采用BEH C18色谱柱(50 mm×2.1 mm,1.7μm),以乙腈-0.1%甲酸水溶液为流动相进行梯度洗脱,流速为0.35 mL·min-1,进样量1μL,柱温45℃,采用电喷雾离子源进行正负离子模式同步检测,多反应监测模式(MRM)用于定量测定。结果:没食子酸、氧化芍药苷、芍药内酯苷、芍药苷、野黄芩苷、灯盏甲素和苯甲酰芍药苷的线性范围分别为2.55～25.48μg·mL-1(r=0.999 3),0.49～4.94μg·mL-1(r=0.994 9),2.02～20.24μg·mL-1(r=0.998 4),6.25～62.52μg·mL-1(r=0.999 2),4.17～41.68μg·mL-1(r=0.997 8),0.17～1.67μg·mL-1(r=0.997 7)和0.80～8.03μg·mL-1(r=0.996 3),其平均回收率分别为98.56%(RSD=2.22%),96.06%(RSD=4.06%),99.27%(RSD=3.79%),98.47%(RSD=0.93%),98.85%(RSD=1.21%),101.03%(RSD=4.69%)和97.69%(RSD=3.71%)。结论:该方法简便,准确,重现性好,专属性高,可用于注射用辛芍(冻干粉针)的质量控制。
OBJECTIVE: To establish an UPLC-MS / MS method for the simultaneous determination of gallic acid, oxycodone, paeoniflorin, paeoniflorin, scutellarin, scutellarin and benzoyl paeoniflorin in injection of Xin Shao MS method. Methods: The gradient elution was performed on a BEH C18 column (50 mm × 2.1 mm, 1.7 μm) with a mobile phase of acetonitrile-0.1% formic acid at a flow rate of 0.35 mL · min -1. The injection volume was 1 μL and the column temperature was 45 ℃, electrospray ionization source was used for synchronous detection of positive and negative ions, and multiple reaction monitoring (MRM) was used for quantitative determination. Results: The linear ranges of gallic acid, paeoniflorin, paeoniflorin, paeoniflorin, scutellarin, scutellarin and benzoyl paeoniflorin were 2.55 ~ 25.48μg · mL -1 (r = 0.999 3) 0.49 to 4.94 μg · mL -1 (r = 0.994 9), 2.02 to 20.24 μg · mL -1 (r = 0.998 4), 6.25 to 62.52 μg · mL -1 (r = 0.999 2), 4.17 to 41.68 μg · (r = 0.997 8), 0.17-1.67 μg · mL-1 (r = 0.997 7) and 0.80- 8.03 μg · mL-1 (r = 0.996 3) .The average recoveries were 98.56% = 2.22%), 96.06% (RSD = 4.06%), 99.27% (RSD = 3.79%), 98.47% (RSD = 0.93%), 98.85% 97.69% (RSD = 3.71%). Conclusion: The method is simple, accurate, reproducible and highly specific. It can be used for the quality control of injection injection of Xin Shao (freeze-dried powder).