UPLC-MS/MS法同时测定降脂活血片中5种成分
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摘要
目的建立超高效液相色谱串联质谱(UPLC-MS/MS)法同时测定降脂活血片(何首乌、黄芪、川芎等)中5种成分的含有量。方法该药物50%甲醇提取液的分析采用Restek UItra Bi Ph色谱柱(100 mm×2.1 mm,5μm);以乙腈(含0.1%甲酸)-0.1%甲酸为流动相,梯度洗脱;体积流量0.4 mL/min;柱温40℃。结果二苯乙烯苷、丹参酮Ⅱ_A、大黄素、阿魏酸、葛根素分别在4.01~1 027、0.73~187、1.48~380、3.98~1 020、4.285~1 097 ng/mL范围内线性关系良好(r>0.994 0),平均加样回收率98.57%~101.0%,RSD(n=6)均小于4.79%。结论该方法专属性强,灵敏度高,可用于降脂活血片的质量控制。
AIM To establish an ultra-performance liquid-chromatography tandem mass spectrometry(UPLCMS/MS) method for the simultaneous content determination of five constituents in Jiangzhi Huoxue Tablets(Polygoni multiflori Radix,Astragali Radix,Chuanxiong Rhizoma,etc.). METHODS The 50% methanol extract of this drug was performed on a 40 ℃ thermostatic Restek UItra Bi Ph column(100 mm × 2. 1 mm,5 μm),with the mobile phase comprising of acetonitrile(containing 0. 1% formic acid)-0. 1% formic acid flowing at 0. 4 mL/min in a gradient elution manner. RESULTS Stilbene glycoside,tanshinoneⅡ_A,emodin,ferulic acid and puerarin showed good linear relationships within the ranges of 4. 01-1 027,0. 7-187,1. 48-380,3. 98-1 020 and4. 285-1 097 ng/mL(r > 0. 994 0),whose average recoveries were 98. 57%-101. 0% with the RSDs(n = 6) of less than 4. 79%. CONCLUSION This specific and sensitive method can be used for the quality control of Jiangzhi Huoxue Tablets.
AIM To establish an ultra-performance liquid-chromatography tandem mass spectrometry(UPLCMS/MS) method for the simultaneous content determination of five constituents in Jiangzhi Huoxue Tablets(Polygoni multiflori Radix,Astragali Radix,Chuanxiong Rhizoma,etc.). METHODS The 50% methanol extract of this drug was performed on a 40 ℃ thermostatic Restek UItra Bi Ph column(100 mm × 2. 1 mm,5 μm),with the mobile phase comprising of acetonitrile(containing 0. 1% formic acid)-0. 1% formic acid flowing at 0. 4 mL/min in a gradient elution manner. RESULTS Stilbene glycoside,tanshinoneⅡ_A,emodin,ferulic acid and puerarin showed good linear relationships within the ranges of 4. 01-1 027,0. 7-187,1. 48-380,3. 98-1 020 and4. 285-1 097 ng/mL(r > 0. 994 0),whose average recoveries were 98. 57%-101. 0% with the RSDs(n = 6) of less than 4. 79%. CONCLUSION This specific and sensitive method can be used for the quality control of Jiangzhi Huoxue Tablets.
引文
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[11]刘自华,安叡,张艺竹,等.HPLC-MS/MS测定葛根芩连汤对大鼠肝脏细胞色素P450酶的影响[J].中国中药杂志,2015,40(15):3072-3080.
[12]王晓明,张帆,刘莹,等.LC-MS/MS法测定升麻中咖啡酸、阿魏酸、异阿魏酸含量的研究[J].天津中医药,2014,31(11):686-689.
[13]刘胜敏,杨志宏,孙晓波,等.LC-MS/MS测定6种丹参主要有效成分及其脑靶向分布研究[J].中国中药杂志,2014,39(9):1704-1708.
[2]姚斌,彭绪坤.降脂活血片治疗脂肪肝130例临床观察[J].中国医药导报,2006,3(29):131-132.
[3]肖昌玉.降脂活血片治疗肥胖症98例[J].实用中医药杂志,2012,28(1):21.
[4]杨久云,张思波.HPLC测定降脂活血片中葛根素的含量[J].中国药师,2007,10(12):1258-1259.
[5]Sun D X,Dong L H,Guo P P,et al.Simultaneous detection of flavonoids and phenolic acids in Herba Lysimachiae and Herba Desmodii Styracifolii using liquid chromatography tandem spectrometry[J].Food Chem,2013,138(1):139-147.
[6]Wang Q,Shi R,Ma Y M,et al.Content determination of the major constituents of Yinchenzhufu decoction via ultra high-performance liquid chromatography coupled with electrospray ionisation tandem mass spectrometry[J].J Pharm Biomed Anal,2013,77:88-93.
[7]Li X,Xiong Z,Ying X,et al.A rapid ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometric method for the qualitative and quantitative analysis of the constituents of the flower of Trollius ledibouri Reichb[J].Anal Chim Acta,2006,580(2):170-180.
[8]孙俊杰.高效液相色谱-质谱联用在药物分析中的应用[D].合肥:中国科学技术大学,2010.
[9]王莹,杜静.液质联用技术在中药复方研究中的应用[J].浙江中西医结合杂志,2015,25(8):799-800.
[10]林佩,陆建美,张光远,等.何首乌活性成分在肝L-02细胞中吸收及代谢产物的LC-MS/MS定性分析[J].中国药学杂志,2015,50(12):1048-1053.
[11]刘自华,安叡,张艺竹,等.HPLC-MS/MS测定葛根芩连汤对大鼠肝脏细胞色素P450酶的影响[J].中国中药杂志,2015,40(15):3072-3080.
[12]王晓明,张帆,刘莹,等.LC-MS/MS法测定升麻中咖啡酸、阿魏酸、异阿魏酸含量的研究[J].天津中医药,2014,31(11):686-689.
[13]刘胜敏,杨志宏,孙晓波,等.LC-MS/MS测定6种丹参主要有效成分及其脑靶向分布研究[J].中国中药杂志,2014,39(9):1704-1708.