HPLC-ESI-MS法同时测定印度獐牙菜中5种酮类化合物的含量 点击下载
论文标题: HPLC-ESI-MS法同时测定印度獐牙菜中5种酮类化合物的含量
英文标题:
中文摘要: 目的:建立同时测定印度獐牙菜中5种 酮类化合物含量的方法。方法:采用高效液相色谱-电喷雾-离子阱质谱(HPLC-ESI-MS)法。色谱条件:色谱柱为Waters Symmetry-C18,流动相为水(5 mmol/L 乙酸铵-0.1%甲酸)-甲醇(梯度洗脱),流速为 0.8 ml/min,检测波长为254 nm,柱温为30 ℃,进样量为10 μl;质谱条件:正离子检测,离子源喷射电压为4.5 kV,毛细管温度为200 ℃,毛细管电压为25 V,鞘气流速为35 arb,辅助气流速为20 arb,碰撞气为氦气,检测方式为多级全扫描质谱。结果:1-羟基-3,5-二甲氧基 酮、1-羟基-3,4,5-三甲氧基 酮、1,8-二羟基-3,5-二甲氧基 酮、1-羟基-2,3,4,5-四甲氧基 酮、1-羟基-2,3,4,7-四甲氧基 酮检测质量浓度线性范围均为0.5~15.00 μg/ml(r均大于0.999 0);精密度、稳定性、重复性试验的RSD<2%;加样回收率分别为100.03%~103.59(RSD=0.99%,n=9)、97.41%~100.89%(RSD=1.15%,n=9)、99.13%~101.68%(RSD=1.40%,n=9)、100.21%~103.51%(RSD=1.33%,n=9)、100.56%~103.92%(RSD=1.37%,n=9)。结论:该方法操作简便,稳定性和重复性好,可用于印度獐牙菜中5 种 酮类化合物含量的同时测定。
英文摘要: OBJECTIVE: To establish a method for the simultaneous determination of 5 xanthones in Swertia chirayita. METHODS: HPLC-EST-MS was conducted. The chromatographic conditions: the column was Waters Symmetry-C18 with mobile phase of water (5 mmol/L ammonium acetate - 0.1% formic acid)-methanol (gradient elution) at a flow rate of 0.8 ml/min, the detection warelength was 254 nm, column temperature was 30 ℃, and the injection volume was 10 μl; MS conditions: it was detected by positive ion, ion source ejection voltage was 4.5 kV, capillary temperature was 200 ℃, capillary voltage was 25 V, sheath gas flow rate was 35 arb, auxiliary gas flow rate was 20 arb, collision gas was helium, and detection method was multi-stage full scan mass spectrometry. RESULTS: The linear ranges for 1-hydroxy-3,5-dimethoxyxanthone,1-hydroxy-3,4,5-trimethoxyxanthone, 1,8-dihydroxy-3,dimethoxyxanthone, 1-hydroxy-2,3,4,5-tetramethoxyxanthone and 1-hydroxy-2,3,4,7-tetramethoxyxanthone were all 0.5-15.00 μg/ml(r>0.999 0); RSDs of precision, stability and reproducibility tests were lower than 2%; recoveries were 100.03%-103.59%(RSD=0.99%,n=9)for 1-hydroxy-3,5-dimethoxyxanthone,97.41%-100.89%(RSD=1.15%,n=9)for 1-hydroxy-3,4,5-trimethoxyxanthone,99.13%-101.68%(RSD=1.40%,n=9)for 1,8-dihydroxy-3,5-dimethoxyxanthone,100.21%-103.51%(RSD=1.33%,n=9)for 1-hydroxy-2,3,4,5-tetramethoxyxanthone,100.56%-103.92%(RSD=1.37%,n=9) for 1-hydroxy-2,3,4,7-tetramethoxyxanthone. CONCLUSIONS: The method is simple, stable and reproducible, and can be used for the simultaneous determination of 5 xanthones in S. chirayita.
期刊: 2016年第27卷第18期
作者: 张大业,陈丽娟,刘健
英文作者: ZHANG Daye,CHEN Lijuan,LIU Jian
关键字: 印度獐牙菜;高效液相色谱法-电喷雾-离子阱质谱法;口(山 )酮
KEYWORDS: Swertia chirayota; HPLC-ESI-MS; Xanthone
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