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目的采用HPLC-MS/MS法同时测定坤复康片中氧化苦参碱、苦参碱、芍药内酯苷、芍药苷及苯甲酰芍药苷等5种有效成分的含量。方法待测样品研磨后采用甲醇超声提取,以Phenomenex Luna C18(150 mm×4.6 mm,5μm)为色谱柱,采用体积分数为0.1%的甲酸乙腈溶液(A)-体积分数为0.1%的甲酸溶液(B)为流动相,梯度洗脱,流速为0.3 m L·min-1,分析时间为9.0 min。质谱ESI源-MRM模式,正、负离子同时检测。5种成分的监测离子对分别为:265.2/247.4(氧化苦参碱)、249.3/148.4(苦参碱)、479.3/197.1(芍药内酯苷)、525.1/121.0(芍药苷)、583.3/120.8(苯甲酰芍药苷)。建立的方法对3批坤复康片进行了测定。结果氧化苦参碱、苦参碱、芍药内酯苷、芍药苷及苯甲酰芍药苷5种有效成分在测定浓度范围内均具有良好的线性关系,r>0.994 8,回收率为95.8%~102.1%。结论用本方法可以同时测定5种有效成分,适用于同时测定坤复康片中氧化苦参碱、苦参碱、芍药内酯苷、芍药苷及苯甲酰芍药苷的含量,同时能较好地控制坤复康片的质量。
OBJECTIVE To determine the contents of 5 active ingredients of kufu Kang Tablets, including oxymatrine, matrine, paeoniflorin, paeoniflorin and paeoniflorin by HPLC-MS / MS. Methods The samples were ground with methanol and then extracted with methanol on a Phenomenex Luna C18 column (150 mm × 4.6 mm, 5 μm) using a 0.1% solution of formic acid in acetonitrile (0.1% in formic acid) (B) as mobile phase, gradient elution at a flow rate of 0.3 m L · min-1 with an analysis time of 9.0 min. Mass spectrometry ESI source-MRM mode, simultaneous detection of positive and negative ions. The monitored ion pairs of the five components were 265.2 / 247.4 (oxymatrine), 249.3 / 148.4 (matrine), 479.3 / 197.1 (paeoniflorin), 525.1 / 121.0 (paeoniflorin), 583.3 / 120.8 (Benzoyl paeoniflorin). The established method of 3 batches of Kun Fu Kang tablets were measured. Results Oxymatrine, matrine, paeoniflorin, paeoniflorin and paeoniflorin in the determination of the five concentrations of active ingredients have a good linear relationship, r> 0.994 8, the recovery rate was 95.8% 102.1%. Conclusions This method can be used to determine the five active ingredients at the same time. It is suitable for the simultaneous determination of oxymatrine, matrine, paeoniflorin, paeoniflorin and paeoniflorin in Kunfukang tablets. To control the quality of Kun Fu Kang tablets.