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目的:建立高效液相色谱-蒸发光散射方法,分析川楝子中柠檬苦素类成分的指纹谱,并测定1-去乙酰基尼泊里宁B的含量。方法:采用YMC-Pack C18(150 mm×4.6 mm,5μm)色谱柱,以流动相甲醇-水-四氢呋喃(55∶40∶5)进行洗脱,流速1.0 mL·min-1,柱温25℃;采用蒸发光散射检测器,漂移管温度93.0℃,载气流速2.3 L·min-1。结果:川楝子中主要含有1-去乙酰基尼泊里宁B(1)、尼泊里宁B(2)、尼泊里宁A(3)、1-顺芷酰基尼泊里宁A(4)、川楝素(5)等柠檬苦素类成分,化合物2~5存在不同程度互变异构现象;1-去乙酰基尼泊里宁B的线性范围为2.324~19.36μg(r=0.9996),平均加样回收率为96.98%,RSD为2.6%。结论:建立的方法符合方法学验证要求,可用于川楝子中柠檬苦素类成分的分析。指纹谱分析结果表明,尼泊里宁型化合物是川楝子中的主要成分;川楝子炮制后指标成分含量有所降低;样品中指标成分含量差异较大。
OBJECTIVE: To establish a HPLC-Evaporative light scattering method to analyze the fingerprints of limonoids in Toosendan sinensis and to determine the content of 1-deacetyl-nalipine B. METHODS: The mobile phase was eluted with methanol-water-tetrahydrofuran (55:40:5) at a flow rate of 1.0 mL · min-1 using a YMC-Pack C18 column (150 mm × 4.6 mm, 5 μm) The evaporating light scattering detector was used. The drift tube temperature was 93.0 ℃ and the carrier gas flow rate was 2.3 L · min-1. Results: Toosendanin mainly contained 1-deacetylnpinazine B (1), nylinine B (2), nylinine A (3), 1- 4) and toosendanin (5). The linear range of 1-deacetyl-niprenin B was 2.324 ~ 19.36μg (r = 0.9996 ), The average recovery was 96.98%, RSD 2.6%. Conclusion: The established method accords with the requirement of methodological verification and can be used to analyze limonoids in Toosendan sinensis. The fingerprinting analysis showed that the neonicotinine compound was the main component of Toosendan sinensis; the content of the index components of Toona sinensis reduced to some extent after processing; the content of the indicator components in the samples differed greatly.