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建立了固相萃取(SPE)-定量核磁共振波谱(qNMR)测定双黄连胶囊中绿原酸含量的方法.绿原酸是双黄连胶囊处方中金银花提取物的有效成分.样品用纯水在室温条件下超声提取,以HC-C18型SPE柱对提取液进行富集净化后,用qNMR测定绿原酸的含量.考察了超声时间、SPE样品前处理条件以及定量核磁共振实验条件对结果的影响.选择氘代二甲基亚砜为溶剂,标定后的对苯二甲醛作为内标.选择脉冲宽度P1=14.1 μs,延迟时间d1=1s,扫描次数NS=512为qNMR定量绿原酸的实验条件.绿原酸的定量峰为δ 6.138-6.182 (H-8',d,1H).结果 显示,所建方法的日内精密度的RSD为1.2％,日间精密度RSD为1.5％,绿原酸与对苯二甲醛峰面积比与质量比的零截距标准曲线线性相关系数为0.9999,且斜率与理论值相符.该法测定绿原酸的LOD为0.0017 mg/g;LOQ为0.079 mg/g.包括样品经SPE预处理过程的绿原酸的回收率为100.2％～103.2％.实际测定双黄连胶囊中的绿原酸的含量为9.68～10.35 mg/g.“,”The determination method of chlorogenic acid in traditional Chinese prescription Shuanghuanglian capsule was established by using quantitative nuclear magnetic resonance spectroscopy (qNMR) in combination with solid phase extraction (SPE).As the capsule's main active component,chlorogenic acid comes from the extraction of Chinese herb medicine Flos Lonicerae.The chlorogenic acid in capsule was ultrasonically extracted at room temperature using pure water as solvent.The extracting solution was enriched and cleaned using HC-C18 SPE cartridge.The effect of ultrasonic extraction,sample pretreatment conditions via SPE and qNMR experimental conditions were investigated.The qNMR experiment conditions were selected using deuterated DMSO as solvent,calibrated 1,4-phthalaldehyde as internal standard,and P1 (pulse width) =14.4 μs,dl (pulse delay time) =1 s,NS (number of scan) =512.The 1H NMR peaks of δ 6.138-6.182 (H-8',d,1H) of chlorogenic acid was chosen as the quantitative peaks.Method validation was performed,including precision (the intra-day RSD =1.2％ and the inter-day RSD =1.5％),linearity (correlation coefficient r＞0.9999),LOD (0.0017 mg/g) and LOQ (0.079 mg/g).The recovery of the SPE-qNMR was within the range of 100.2％-103.2％.The result showed that the method was stable,accurate and reliabile.Determined by the method,the chlorogenic acid in a real Shuanghuanglian capsule was within the range of 9.68-10.35 mg/g.