超高效液相色谱质谱联用技术快速检测中药钩藤中6种钩藤碱含量
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摘要
目的建立UPLC-MS/MS方法测定中药钩藤中钩藤碱、异钩藤碱、去氢钩藤碱、异去氢钩藤碱、毛钩藤碱与去氢毛钩藤碱含量。方法以地西泮为内标,采用UPLC BEH(2. 1 mm×50 mm,1. 7μm)柱,柱温为40℃。流动相由乙腈和水(含0. 1%甲酸)组成,梯度洗脱流速为0. 4 ml/min,洗脱时间为5. 5 min。MRM模式对钩藤碱、异钩藤碱、去氢钩藤碱、异去氢钩藤碱、毛钩藤碱与去氢毛钩藤碱进行定量分析。蒸馏水煮法对中药钩藤进行提取。结果在0. 005μg/ml～5μg/ml浓度时,钩藤碱、异钩藤碱、去氢钩藤碱、异去氢钩藤碱、毛钩藤碱与去氢毛钩藤碱线性良好(r> 0. 995),最低定量下限为0. 005μg/ml。日内精密度RSD≤8%,日间精密度RSD≤10%。准确度在93. 4%～108. 7%。结论该分析方法灵敏、快速、选择性好,并成功应用于中药钩藤中钩藤碱、异钩藤碱、去氢钩藤碱、异去氢钩藤碱、毛钩藤碱与去氢毛钩藤碱含量测定。
Objective An ultra performance liquid chromatography tandem mass spectrometry( UHPLC-MS/MS) method was established for the determination of rhynchophylline,isorhynchophylline,corynoxeine,isocorynoxeine,hirsutine and hirsuteine in Uncaria Rhynchophylla. Methods With diazepam as internal standard,UPLC BEH( 2. 1 mm × 50 mm,1. 7 μm) column was used for chromatographic separation and the column temperature was set at 40 °C. A binary gradient consisting of acetonitrile and 0. 1% formic acid was employed over 5. 5 min with a gradient elution flow rate at 0. 4 ml/min. MRM model was used for the quantitative analysis of rhynchophylline,isorhynchophylline,corynoxeine,isocorynoxeine,hirsutine and hirsuteine.Distilled water was used to extract the Chinese herbal Uncaria Rhynchophylla. Results In the concentration of 0. 005 μg/ml-5 μg/ml,rhynchophylline,isorhynchophylline,corynoxeine,isocorynoxeine,hirsutine and hirsuteine were linear( r > 0. 995);the lower limit of quantitation was 0. 005 μg/ml. Intra-day precision RSD was not more than 8%,inter-day precision RSD was not more than 10%. The accuracy was within 93. 4%-108. 7%. Conclusion The method was sensitive,rapid,and selectivity. It has been successfully applied to the determination of rhynchophylline,isorhynchophylline,corynoxeine,isocorynoxeine,hirsutine and hirsuteine in Uncaria Rhynchophylla.
Objective An ultra performance liquid chromatography tandem mass spectrometry( UHPLC-MS/MS) method was established for the determination of rhynchophylline,isorhynchophylline,corynoxeine,isocorynoxeine,hirsutine and hirsuteine in Uncaria Rhynchophylla. Methods With diazepam as internal standard,UPLC BEH( 2. 1 mm × 50 mm,1. 7 μm) column was used for chromatographic separation and the column temperature was set at 40 °C. A binary gradient consisting of acetonitrile and 0. 1% formic acid was employed over 5. 5 min with a gradient elution flow rate at 0. 4 ml/min. MRM model was used for the quantitative analysis of rhynchophylline,isorhynchophylline,corynoxeine,isocorynoxeine,hirsutine and hirsuteine.Distilled water was used to extract the Chinese herbal Uncaria Rhynchophylla. Results In the concentration of 0. 005 μg/ml-5 μg/ml,rhynchophylline,isorhynchophylline,corynoxeine,isocorynoxeine,hirsutine and hirsuteine were linear( r > 0. 995);the lower limit of quantitation was 0. 005 μg/ml. Intra-day precision RSD was not more than 8%,inter-day precision RSD was not more than 10%. The accuracy was within 93. 4%-108. 7%. Conclusion The method was sensitive,rapid,and selectivity. It has been successfully applied to the determination of rhynchophylline,isorhynchophylline,corynoxeine,isocorynoxeine,hirsutine and hirsuteine in Uncaria Rhynchophylla.
引文
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[15]黄爱芳,李建波,冯露敏,等. LC-MS法同时检测人血浆中杜冷丁、曲马多和美沙酮[J].中国卫生检验杂志,2010,20(12):3191-3192.
[16]王贤亲,林丹,潘晓军,等. LC-APCI-M/SMS测定全血中苯妥英钠的含量[J].中国卫生检验杂志,2008,18(12):2455-2456,2511.
[17]王贤亲,林丹,李艳霞,等. LC-M/SMS测定人血浆中5种有机磷的含量[J].中国卫生检验杂志,2008,18(12):2537-2539.
[18]魏华琳,蒋培,陶健.高效液相色谱-串联质谱法测定粉状化妆品中氟轻松[J].中国卫生检验杂志,2017,27(24):3526-3528.
[19]裴昆,刘荷英,左丽平,等.液相色谱-串联质谱法同时检测消字号产品中的地塞米松和氯倍他索丙酸酯[J].中国卫生检验杂志,2017,27(21):3071-3073,3076.
[20]康莉,刘红河,廖仕成,等.电喷雾液相色谱串联质谱法测定人尿中10种邻苯二甲酸单酯[J].中国卫生检验杂志,2017,27(23):3349-3351,3356.
[21]胡立成,朱传新.尿液中典型胆汁酸的超高效液相色谱-串联三重四级杆质谱分析方法[J].中国卫生检验杂志,2017,27(24):3523-3525,3528.
[2]崔莹.钩藤化学成分和药理活性研究进展[J].西安文理学院学报:自然科学版,2015,18(4):16-18.
[3]王章姐,孙维矿.钩藤的化学成分及药理作用研究进展[J].现代企业教育,2010,371(24):197-198.
[4]田玲,姚成,边敏.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[J].理化检验:化学分册,2018,54(2):138-141.
[5]尚艳玲.高效液相色谱-蒸发散射检测器法测定中药钩藤中钩藤碱的含量[J].黑龙江科技信息,2015(20):69.
[6]曾启华,李森柱,王蒙,等. HPLC法对钩藤超临界萃取物中钩藤碱的分析[J].湖北农业科学,2015,54(21):5398-5400.
[7]何红晖.钩藤药材中异钩藤碱含量的超高效液相色谱和高效液相色谱法的测定[J].中国医药指南,2015,13(21):62-63.
[8]邓岳,刘阿娜,王小明,等. UPLC法同时测定钩藤提取物中4种生物碱类成分的含量[J].中药材,2016,39(4):819-821.
[9]池雨锋,王小明,张玲,等. HPLC-MS法同时测定钩藤药材中四种生物碱含量[J].山东中医药大学学报,2017,41(3):262-265.
[10] Zhang WM,Li RF,Sun M,et al. UPLC-MS/MS method for determination of avicularin in rat plasma and its application to a pharmacokinetic study[J]. J Chromatogr B,2014,965:107-111.
[11] Wang Z,Yang H,Sun W,et al. UPLC-MS/MS determination of thiamphenicol in human plasma and its application to a pharmacokinetic study[J]. J Chromatogr B,2014,967:235-239.
[12] Gadgil P,Ibrahim F,Chow DS. UPLC-MS/MS assay of 21-aminosteroid(lazaroid U74389G)for application in pharmacokinetic study[J]. J Pharmaceut Biomed,2016,122:90-97.
[13]杨学志,陈国钱,王贤亲,等. LC-ESI-MS测定人血浆中丙戊酸钠浓度[J].中国卫生检验杂志,2010,20(6):1356-1357,1451.
[14]林观样,王贤亲,胡卢丰. LC-ESI-MS测定人血浆中的姜黄素[J].中国卫生检验杂志,2010,20(4):756-757.
[15]黄爱芳,李建波,冯露敏,等. LC-MS法同时检测人血浆中杜冷丁、曲马多和美沙酮[J].中国卫生检验杂志,2010,20(12):3191-3192.
[16]王贤亲,林丹,潘晓军,等. LC-APCI-M/SMS测定全血中苯妥英钠的含量[J].中国卫生检验杂志,2008,18(12):2455-2456,2511.
[17]王贤亲,林丹,李艳霞,等. LC-M/SMS测定人血浆中5种有机磷的含量[J].中国卫生检验杂志,2008,18(12):2537-2539.
[18]魏华琳,蒋培,陶健.高效液相色谱-串联质谱法测定粉状化妆品中氟轻松[J].中国卫生检验杂志,2017,27(24):3526-3528.
[19]裴昆,刘荷英,左丽平,等.液相色谱-串联质谱法同时检测消字号产品中的地塞米松和氯倍他索丙酸酯[J].中国卫生检验杂志,2017,27(21):3071-3073,3076.
[20]康莉,刘红河,廖仕成,等.电喷雾液相色谱串联质谱法测定人尿中10种邻苯二甲酸单酯[J].中国卫生检验杂志,2017,27(23):3349-3351,3356.
[21]胡立成,朱传新.尿液中典型胆汁酸的超高效液相色谱-串联三重四级杆质谱分析方法[J].中国卫生检验杂志,2017,27(24):3523-3525,3528.