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目的:建立UPLC法同时测定青海川西獐牙菜中獐牙菜苦苷、龙胆苦苷、獐牙菜苷、芒果苷、异荭草苷和异牡荆素6个主要有效成分的含量。方法:使用ASE 350快速溶剂萃取仪(ASE)通过在线净化过程用甲醇提取出样品中的6个主要有效成分,分析物的色谱分离采用Endeavorsil-C18色谱柱(2.1 mm×100 mm,1.8μm),以甲醇-0.1%乙酸水溶液为流动相梯度洗脱,流速为0.2 m L·min~(-1),室温下进行试验,检测波长为260 nm。结果:獐牙菜苦苷、龙胆苦苷、獐牙菜苷、芒果苷、异荭草苷和异牡荆素的进样浓度分别在0.510 9~40.87 mg·L~(-1)(r=0.999 2)、1.633~130.7 mg·L~(-1)(r=0.999 9)、0.679 0~54.32 mg·L~(-1)(r=0.999 0)、0.470 0~37.60 mg·L~(-1)(r=0.999 0)、0.281 8~22.54 mg·L~(-1)(r=0.999 2)、0.223 0~17.84 mg·L~(-1)(r=0.999 3)范围内与峰面积呈良好的线性;平均加样回收率(n=9)均在96.4%~100.1%范围内,RSD均在1.1%~2.6%范围内。10批样品中各成分含量(n=3)分别为獐牙菜苦苷1.46~9.17 mg·g~(-1),龙胆苦苷7.31~16.84 mg·g~(-1),獐牙菜苷1.72~7.22 mg·g~(-1),芒果苷3.39~8.88 mg·g~(-1),异荭草苷1.35~5.31 mg·g~(-1),异牡荆素0.06~0.34 mg·g~(-1)。结论:该方法可用于川西獐牙菜中上述6种主要有效成分的含量测定,为青海川西獐牙菜的质量控制提供依据。
OBJECTIVE: To establish a UPLC method for the simultaneous determination of swertia glycosides, gentiopicroside, swertia glycosides, mangiferin, isoorientin and isovitamin in six species of Swertia sinensis in Qinghai. Methods: Six major active ingredients of the sample were extracted with methanol using an ASE 350 Fast Solvent Extractor (ASE). The chromatographic separation of the analytes was performed on an Endeavorsil-C18 column (2.1 mm × 100 mm, 1.8 μm) The mobile phase was eluted with methanol-0.1% acetic acid aqueous solution at a flow rate of 0.2 mL · min -1. The detection wavelength was 260 nm at room temperature. Results: The injection concentrations of swertia glycosides, gentiopicroside, swertiacein, mangiferin, isoorientin and isovitamin were 0.510 9-40.87 mg · L -1 (r = 0.999 2), 1.633 ~ 130.7 mg · L -1 (r = 0.999 9), 0.679 0 ~ 54.32 mg · L -1 (r = 0.999 0), 0.470 0 ~ 37.60 mg · L -1 (R = 0.999 0), 0.281 8 ~ 22.54 mg · L -1 (r = 0.999 2) and 0.223 0 ~ 17.84 mg · L -1 (r = 0.999 3) (N = 9) were in the range of 96.4% ~ 100.1%, and the RSDs were in the range of 1.1% ~ 2.6%. The contents of each component in 10 batches of samples (n = 3) were 1.46-9.17 mg · g -1 for swertia glycosides, 7.31-16.84 mg · g -1 for gentiopicroside, 1.72 ~ 7.22 mg · g ~ (-1), 3.39 ~ 8.88 mg · g ~ (-1) for mangiferin, 1.35 ~ 5.31 mg · g ~ (-1) for isoorientin and 0.06 ~ 0.34 mg · g ~ (-1). Conclusion: The method can be used for the determination of the above six active ingredients in Swertia chuanxxi and provide the basis for the quality control of Swertia.