目的 建立定量核磁共振技术(qNMR)同时测定注射用丹参多酚酸中咖啡酸、丹参素、原儿茶酸和阿魏酸。方法 通过qNMR测定4种单体酚酸，脉冲序列^zg30抑制水峰，谱宽设定8 012.8 Hz，温度为25℃，采样点数为131 072，采集时间为4.09 s，弛豫延迟时间为8.26 s，纵向弛豫时间为1.25 s；采样次数为16，接收器增益值为35.6，数字化仪分辨率值为18，空扫次数为4，发射机频率偏移为6.0×10^-6。以三氟乙酸-d为内标，根据峰面积比与质量比计算4种单体酚酸的含量。结果 咖啡酸、丹参素、原儿茶酸、阿魏酸分别选取9.47×10^-6(s，H-7)、8.02×10^-6(s，H-8)、5.86×10^-6(s，H-8)、12.79×10^-6(s，H-8)处的信号为定量峰；分析物在12 h后稳定性较差，所有样品在制备后12 h内完成测定；咖啡酸在0.103～1.625 μg·mL^-1(r²=0.999 3)，丹参素在2.256～3.194 μg·mL^-1(r²=0.999 5)，原儿茶酸在9.699～13.584 μg·mL^-1(r²=0.999 8)，阿魏酸在1.566～2.649 μg·mL^-1(r²=0.999 6)均呈良好的线性关系；加样回收率分别为104.9%、101.5%、104.1%、101.4%，RSD值分别为1.6%、2.1%、2.3%、1.5%；精密度、准确性、重复性均良好。结论 建立的qNMR可同时测定注射用丹参多酚酸中咖啡酸、丹参素、原儿茶酸和阿魏酸。

Objective To establish a quantitative nuclear magnetic resonance (qNMR) technique for the simultaneous determination of caffeic acid, danshensu, protocatechuic acid and ferulic acid in Salvianolic Acids for Injection. Methods The contents of phenolic acids in four monomers were determined by qNMR. Pulse sequence ^zg30 suppresses water peaks, with a spectral width set to 8 012.8 Hz, temperature was 25 ℃, sampling points are 131 072, collection time was 4.09 s, relaxation delay time was 8.26 s, and longitudinal relaxation time was 1.25 s. The sampling frequency was 16, the receiver gain value was 35.6, the digitizer resolution value was 18, the number of spatial scans was 4, and the transmitter frequency offset was 6.0 × 10^-6. The contents of phenolic acids in four monomers were calculated according to the integral peak area ratio and mass ratio with trifluoroacetic acid-d as the internal standard. Results The signal for caffeic acid, danshensu, protocatechuic acid and ferulic acid was 9.47×10^-6(s, H-7), 8.02×10^-6(s, H-8), 5.86× 10^-6(s, H-8), and 12.79×10^-6(s, H-8) respectively. Caffeic acid ranged from 0.103-1.625 μg·mL^-1 (r²=0.999 3), danshensu ranged from 2.256-3.194 μg·mL^-1 (r²=0.999 5), protocatechuic acid ranged from 9.699-13.584 μg·mL^-1 (r²=0.999 8), ferulic acid ranged from 1.566-2.649 μg·mL^-1 (r²=0.999 6). The recoveries were 104.9%, 101.5%, 104.1% and 101.4% respectively, and the RSD values were 1.6%, 2.1%, 2.3% and 1.5% respectively. The precision, accuracy, and repeatability are all good. Conclusion qNMR can simultaneously determine the contents of four monomeric phenolic acids in Salvianolic Acids for Injection.

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