目的 建立定量核磁共振技術(shù)(qNMR)同時(shí)測定注射用丹參多酚酸中咖啡酸、丹參素、原兒茶酸和阿魏酸。方法 通過qNMR測定4種單體酚酸，脈沖序列^zg30抑制水峰，譜寬設(shè)定8 012.8 Hz，溫度為25℃，采樣點(diǎn)數(shù)為131 072，采集時(shí)間為4.09 s，弛豫延遲時(shí)間為8.26 s，縱向弛豫時(shí)間為1.25 s；采樣次數(shù)為16，接收器增益值為35.6，數(shù)字化儀分辨率值為18，空掃次數(shù)為4，發(fā)射機(jī)頻率偏移為6.0×10^-6。以三氟乙酸-d為內(nèi)標(biāo)，根據(jù)峰面積比與質(zhì)量比計(jì)算4種單體酚酸的含量。結(jié)果 咖啡酸、丹參素、原兒茶酸、阿魏酸分別選取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)處的信號為定量峰；分析物在12 h后穩(wěn)定性較差，所有樣品在制備后12 h內(nèi)完成測定；咖啡酸在0.103～1.625 μg·mL^-1(r²=0.999 3)，丹參素在2.256～3.194 μg·mL^-1(r²=0.999 5)，原兒茶酸在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)均呈良好的線性關(guān)系；加樣回收率分別為104.9%、101.5%、104.1%、101.4%，RSD值分別為1.6%、2.1%、2.3%、1.5%；精密度、準(zhǔn)確性、重復(fù)性均良好。結(jié)論 建立的qNMR可同時(shí)測定注射用丹參多酚酸中咖啡酸、丹參素、原兒茶酸和阿魏酸。

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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