以离子液体为流动相添加剂的高效液相色谱法测定钩藤药材中钩藤碱和异钩藤碱
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摘要
采用以离子液体为流动相添加剂的高效液相色谱法测定钩藤药材中钩藤碱和异钩藤碱的含量。钩藤药材样品0.532g用60%(体积分数)甲醇溶液10mL在25℃下超声提取30min。过滤后的续滤液以C18色谱柱为分离柱,以16.7 mmol·L~(-1)磷酸二氢钾缓冲溶液(pH 3.0,20mmol·L~(-1) 1-己基-3-甲基咪唑四氟硼酸盐离子液体作为添加剂)为流动相,在检测波长245nm处进行测定。钩藤碱与异钩藤碱的质量浓度均在1.56~100mg·L~(-1)内与其对应的峰面积呈线性关系,检出限(3S/N)依次为0.914,0.194 mg·L~(-1)。方法用于钩藤药材样品的分析,回收率为98.0%~101%,测定值的相对标准偏差(n=6)为0.60%~1.8%。
HPLC was applied to the determination of rhychophylline and isorhychophylline in uncaria with ionic liquid as mobile phase additive.The uncaria sample(0.532 g)was extracted ultrasonically with 60%(φ)methanol solution(10 mL)for 30 min at 25 ℃.After filtration,subsequent filtrate was collected.C_(18) chromatographic column was used as stationary phase,and buffer solution of 16.7 mmol·L~(-1) KH_2PO_4(pH 3.0,20 mmol·L~(-1)[HMIM][BF_4]ionic liquid used as additive)was used as mobile phase.UV-detection at 245 nm was adopted in the determination.Linear relationships between values of peak area and mass concentration of rhychophylline and isorhychophylline were kept in the same range of 1.56~(-1)00 mg·L~(-1),with detection limits(3 S/N)of 0.914,0.194 mg·L~(-1),respectively.The proposed method was applied to the analysis of the sample of uncaria,giving values of recovery and RSD′s(n=6)in the ranges of 98.0%~(-1)01% and 0.60%~(-1).8%,respectively.
HPLC was applied to the determination of rhychophylline and isorhychophylline in uncaria with ionic liquid as mobile phase additive.The uncaria sample(0.532 g)was extracted ultrasonically with 60%(φ)methanol solution(10 mL)for 30 min at 25 ℃.After filtration,subsequent filtrate was collected.C_(18) chromatographic column was used as stationary phase,and buffer solution of 16.7 mmol·L~(-1) KH_2PO_4(pH 3.0,20 mmol·L~(-1)[HMIM][BF_4]ionic liquid used as additive)was used as mobile phase.UV-detection at 245 nm was adopted in the determination.Linear relationships between values of peak area and mass concentration of rhychophylline and isorhychophylline were kept in the same range of 1.56~(-1)00 mg·L~(-1),with detection limits(3 S/N)of 0.914,0.194 mg·L~(-1),respectively.The proposed method was applied to the analysis of the sample of uncaria,giving values of recovery and RSD′s(n=6)in the ranges of 98.0%~(-1)01% and 0.60%~(-1).8%,respectively.
引文
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[9]边敏,杨勇.以离子液体为流动相添加剂高效液相色谱法分离季铵型生物碱[J].分析科学学报,2013,29(6):791-795.
[10]FLIEGER J,SWIEBODA R.Application of chaotropic effect in reversed-phase liquid chromatography of structurally related phenothiazine and thioxanthene derivatives[J].Journal of Chromatography A,2008,1192(2):218-224.
[11]BIAN M,ZHANG Z J,YIN H J.Effects and mechanism characterization of ionic liquids as mobile phase additives for separation of matrine-type alkaloids by liquid chromatography[J].Journal of Pharmaceutical and Biomedical Analysis,2012,58(25):163-167.
[12]TOKUDA H,HAYAMIZU K,ISHII K.Physicochemical properties and structures of room temperature ionic liquids.2.variation of alkyl chain length in imidazolium cation[J].Journal of Physical Chemistry B,2005,109(13):6103-6110.
[13]WU Z F,WANG Y Q,WAN N,et al.Structural stabilitie and transformation mechanism of rhynchophylline and isorhynchophylline by ultra performance liquid chromatography/time-of-flight mass spectrometry(UPLC/Q-TOF-MS)[J].Molecules,2015,20(8):14849-14859.
[2]赵晓丽,马艳.HPLC法测定钩藤中钩藤碱和异钩藤碱含量[J].中国医药科学,2013,3(13):97-98.
[3]王义祥,侍媛媛,解双陆,等.钩藤吲哚类生物碱分析方法研究进展[J].医药进展,2013,37(6):257-264.
[4]WU Y T,LIN L C,TSAI T H.Determination of rhynchophylline and hirsutine in rat plasma by UPLCMS/MS after oral administration of Uncaria rhynchophylla extract[J].Biomedical Chromatography,2014,28(3):439-445.
[5]ZHOU J Y,ZHOU S W.Isorhynchophylline:A plant alkaloid with therapeutic potential for cardiovascular and central nervous system diseases[J].Fitoterapia,2012,83(4):617-626.
[6]汪江涛,丁伯平.钩藤碱和异钩藤碱药理作用研究进展[J].中国医药指导,2012,14(7):1224-1225.
[7]罗由萍,邓鹏飞.薄层色谱及其在药用植物研究中的作用[J].安徽农业科学,2011,39(6):3309-3312.
[8]边敏,杨勇,周昊.以离子液体作流动相添加剂高效液相色谱法分离辣椒素类生物碱[J].分析测试学报,2013,32(2):174-178.
[9]边敏,杨勇.以离子液体为流动相添加剂高效液相色谱法分离季铵型生物碱[J].分析科学学报,2013,29(6):791-795.
[10]FLIEGER J,SWIEBODA R.Application of chaotropic effect in reversed-phase liquid chromatography of structurally related phenothiazine and thioxanthene derivatives[J].Journal of Chromatography A,2008,1192(2):218-224.
[11]BIAN M,ZHANG Z J,YIN H J.Effects and mechanism characterization of ionic liquids as mobile phase additives for separation of matrine-type alkaloids by liquid chromatography[J].Journal of Pharmaceutical and Biomedical Analysis,2012,58(25):163-167.
[12]TOKUDA H,HAYAMIZU K,ISHII K.Physicochemical properties and structures of room temperature ionic liquids.2.variation of alkyl chain length in imidazolium cation[J].Journal of Physical Chemistry B,2005,109(13):6103-6110.
[13]WU Z F,WANG Y Q,WAN N,et al.Structural stabilitie and transformation mechanism of rhynchophylline and isorhynchophylline by ultra performance liquid chromatography/time-of-flight mass spectrometry(UPLC/Q-TOF-MS)[J].Molecules,2015,20(8):14849-14859.