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目的:采用高效液相色谱法同时测定藏药独一味及其伪品糙苏中胡麻属苷、山栀苷甲酯、绿原酸、8-O-乙酰山栀苷甲酯、连翘酯苷B、木犀草苷和毛蕊花糖苷7个成分的含量,并比较两者成分的差异。方法:采用HSS T3 C18色谱柱(4.6 mm×250 mm,5μm),以乙腈(A)-0.1%磷酸水溶液(B)为流动相,梯度洗脱(0~11 min,9%A;11~35 min,9%A→18%A;35~50 min,18%A),流速1.0 mL·min~(-1),检测波长为235 nm,柱温30℃。结果:50 min内独一味和糙苏的主要色谱峰能够达到完全分离,胡麻属苷、山栀苷甲酯、绿原酸、8-O-乙酰山栀苷甲酯、连翘酯苷B、木犀草苷和毛蕊花糖苷质量浓度分别在2.026~81.04μg·mL~(-1)(r=0.999 9,n=6)、2.064~82.56μg·mL~(-1)(r=0.999 9,n=6)、1.924~96.20μg·mL~(-1)(r=0.999 8,n=6)、1.912~76.48μg·mL~(-1)(r=0.999 9,n=6)、1.874~74.96μg·mL~(-1)(r=0.999 8,n=6)、1.948~77.92μg·mL~(-1)(r=0.999 9,n=6)和1.890~75.60μg·mL~(-1)(r=0.999 9,n=6)范围内线性关系良好。11批独一味中胡麻属苷、山栀苷甲酯、绿原酸、8-O-乙酰山栀苷甲酯、连翘酯苷B、木犀草苷和毛蕊花糖苷含量范围范围分别为0.265%~0.872%、0.354%~1.058%、0.124%~0.641%、0.182%~1.426%、0.121%~0.719%、0.138%~1.301%和0.091%~1.173%;12批糙苏中胡麻属苷、山栀苷甲酯、8-O-乙酰山栀苷甲酯、连翘酯苷B和毛蕊花糖苷含量范围分别为0.196%~0.751%、0.358%~0.652%、0.204%~0.822%、0.101%~0.761%和0.024%~0.682%,均未检出绿原酸和木犀草苷。结论:所建立方法操作简单,具有较好的重复性和稳定性,结合伪品的同时测定,可用于独一味药材的质量控制。
OBJECTIVE: To simultaneously determine the contents of flaxseed glycosides, methylhomoside, chlorogenic acid, 8-O-acetylglucoside methyl ester, forsythiaside B, luteolin and verbascoside seven components, and compare the differences between the two components. Methods: The mobile phase was eluted with gradient elution (0 ~ 11 min, 9% A, 11 ~ 10 min) using HSS T3 C18 column (4.6 mm × 250 mm, 35 min, 18 min, 35 min, 18 min). The flow rate was 1.0 mL · min -1. The detection wavelength was 235 nm and the column temperature was 30 ℃. Results: The main chromatographic peaks of monosodium glutamate and pyronin in 50 min were completely separated. Flax glycosides, methylhomoside, chlorogenic acid, 8-O-acetylglucoside methyl ester, forsythiaside B, The concentrations of luteolin and verbascoside were 2.026 ~ 81.04μg · mL -1 (r = 0.999 9, n = 6), 2.064 ~ 82.56μg · mL -1 (r = 0.999 9, n (R = 0.999 8, n = 6), 1.912 ~ 76.48μg · mL -1 (r = 0.999 9, n = 6) and 1.874 ~ (R = 0.999 8, n = 6), 1.948 ~ 77.92μg · mL -1 (r = 0.999 9, n = 6) and 1.890 ~ 75.60μg · mL -1 -1) (r = 0.999 9, n = 6) within a good linear relationship. 11 batches of flavors of flax glycosides, inosine methyl ester, chlorogenic acid, 8-O-acetylglucoside methyl ester, forsythoside B, luteolin and verbascoside content range of 0.265% 0.872%, 0.354% ~ 1.058%, 0.124% ~ 0.641%, 0.182% ~ 1.426%, 0.121% ~ 0.719%, 0.138% ~ 1.301% and 0.091% ~ 1.173% The content of glycoside methyl ester, 8-O-acetylglucoside methyl ester, forsythiaside B and verbascoside range from 0.196% to 0.751%, 0.358% to 0.652%, 0.204% to 0.822%, 0.101% to 0.761% And 0.024% -0.682%, respectively. No chlorogenic acid and luteolin were detected. Conclusion: The established method is simple, has good repeatability and stability, combined with the simultaneous determination of counterfeit products, can be used for the quality control of the only flavor herbs.