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目的:HPLC波长切换联合梯度洗脱法同时测定荆防败毒丸中的5-O-咖啡酰莽草酸、落新妇苷、花旗松素、黄杞苷、白藜芦醇、洋川芎内酯H、洋川芎内酯I、洋川芎内酯A、瑟丹酸内酯和藁本内酯含量。方法:采用Shiseido C_(18)色谱柱(4.6 mm×250 mm,5μm),以甲醇-乙腈(3∶1)(A)与0.1%冰醋酸水溶液(B)为流动相,梯度洗脱,流速1.2mL·min~(-1),柱温30℃,5-O-咖啡酰莽草酸、落新妇苷、花旗松素、黄杞苷和白藜芦醇的检测波长为291 nm,洋川芎内酯H、洋川芎内酯I、洋川芎内酯A、瑟丹酸内酯和藁本内酯的检测波长为280 nm。结果:5-O-咖啡酰莽草酸、落新妇苷、花旗松素、黄杞苷、白藜芦醇、洋川芎内酯H、洋川芎内酯I、洋川芎内酯A、瑟丹酸内酯和藁本内酯10个成分的线性范围分别为9.13~182.60μg·mL~(-1)(r=0.999 4)、20.75~415.00μg·mL~(-1)(r=0.999 9)、3.54~70.80μg·mL~(-1)(r=0.999 5)、4.78~95.60μg·mL~(-1)(r=0.999 8)、2.42~48.40μg·mL~(-1)(r=0.999 3)、3.38~67.60μg·mL~(-1)(r=0.999 9)、4.94~98.80μg·mL~(-1)(r=0.999 6)、6.36~127.20μg·mL~(-1)(r=0.999 8)、3.07~61.40μg·mL~(-1)(r=0.999 7)、9.66~193.20μg·mL~(-1)(r=0.999 5);平均加样回收率(n=6)分别为97.3%(RSD=1.1%)、99.2%(RSD=1.3%)、96.8%(RSD=0.44%)、98.8%(RSD=0.86%)、96.9%(RSD=1.1%)、98.3%(RSD=1.6%)、97.1%(RSD=1.2%)、100.0%(RSD=0.60%)、97.9%(RSD=1.3%)、99.2%(RSD=1.1%)。3批样品中上述10个成分的含量范围分别为0.542~0.579、1.519~1.663、0.105~0.117、0.314~0.331、0.072~0.081、0.101~0.113、0.164~0.183、0.406~0.437、0.163~0.182、0.585~0.607 mg·g~(-1)。结论:本文建立的HPLC波长切换联合梯度洗脱法可为荆防败毒丸质量标准的提高提供依据。
OBJECTIVE: Simultaneous determination of 5-O-caffeoylshikimate, astilbin, taxifolin, flavonoid, resveratrol, and yangchongxiong lactone in Jingfubudu pill by HPLC wavelength switching combined with gradient elution , Rhizoma Chuanxiong I, Rhizoma Chuanxiong A, cortex lactone and ligustilide. Methods: The mobile phase was eluted with a mobile phase of Shiseido C 18 column (4.6 mm × 250 mm, 5 μm) with methanol-acetonitrile (3:1) (A) and 0.1% 1.2mL · min -1, the column temperature was 30 ℃. The detection wavelength of 5-O-caffeoyl shikimic acid, astilbin, taxifolin, flavonoid and resveratrol was 291 nm. The detection wavelength of the ester H, the yangchongxiong I, the yangchongxiong A, the cydanilide and the ligustilide were 280 nm. Results: 5-O-caffeoyl shikimic acid, astilbin, taxifolin, huang glycoside, resveratrol, oriental rhizoma ligusticin H, oriental rhizoma ligustici I, The linear range of the ten components of esters and ligustilide were 9.13 ~ 182.60μg · mL -1 (r = 0.999 4), 20.75 ~ 415.00μg · mL -1 (r = 0.999 9), (R = 0.999 5), 4.78 ~ 95.60 μg · mL -1 (r = 0.999 8), 2.42 ~ 48.40 μg · mL -1 (r = 0.999 3), 3.38 ~ 67.60μg · mL -1 (r = 0.999 9), 4.94 ~ 98.80μg · mL -1 (r = 0.999 6), 6.36 ~ 127.20μg · mL -1 (r = 0.999 8), 3.07 ~ 61.40μg · mL -1 (r = 0.999 7) and 9.66 ~ 193.20μg · mL -1 (r = 0.999 5) 99.8% (RSD = 1.3%), 96.8% (RSD = 0.44%), 98.8% (RSD = 0.86%) and 96.9% (RSD = 1.1% , 98.3% (RSD = 1.6%), 97.1% (RSD = 1.2%), 100.0% (RSD = 0.60%), 97.9% (RSD = 1.3%), 99.2% (RSD = 1.1%). The contents of the above 10 components in three batches of samples ranged from 0.542 to 0.579, from 1.519 to 1.663, from 0.105 to 0.117, from 0.314 to 0.331, from 0.072 to 0.081, from 0.101 to 0.113, from 0.164 to 0.183, from 0.406 to 0.437, from 0.163 to 0.182, ~ 0.607 mg · g ~ (-1). Conclusion: The combination of HPLC wavelength shift and gradient elution method established in this paper can provide the basis for improving the quality standard of Jing Fang Baoxin capsule.