UPLC-ESI-MS法同时测定苗药红禾麻中11个成分的含量

目的：建立超高效液相色谱-串联质谱（UPLC-ESI-MS）法同时测定苗药红禾麻中没食子儿茶素、新绿原酸、表没食子儿茶素、儿茶素、绿原酸、隐绿原酸、表儿茶素、芦丁、异槲皮苷、山柰酚-3-O-芸香糖苷、槲皮苷11个成分的含量。方法：采用ACQUITY UPLC BEH C₁₈色谱柱（2.1 mm×100 mm，1.7μm），以0.1%甲酸水溶液-0.1%甲酸乙腈溶液为流动相，梯度洗脱，流速0.25 mL·min^-1，柱温45℃，采用电喷雾离子源（ESI），选择离子监测（SIM）模式检测。结果：没食子儿茶素、新绿原酸、表没食子儿茶素、儿茶素、绿原酸、隐绿原酸、表儿茶素、芦丁、异槲皮苷、山柰酚-3-O-芸香糖苷、槲皮苷的质量浓度分别在0.051~3.256、0.050~3.200、0.056~3.594、0.050~3.206、0.109~6.975、0.053~3.394、0.012~3.087、0.012~50.800、0.026~3.363、0.065~26.550、0.013~3.328 mg·L^-1范围内与峰面积呈良好线性关系，R²均大于0.9990，平均加样回收率在94%~103%范围内。13批样品中没食子儿茶素、新绿原酸、表没食子儿茶素、儿茶素、绿原酸、隐绿原酸、表儿茶素、芦丁、异槲皮苷、山柰酚-3-O-芸香糖苷、槲皮苷的含量测定结果分别为2.00~27.45、2.41~20.76、1.63~27.57、1.75~20.80、16.35~115.81、4.28~20.04、0.48~17.41、102.90~935.53、9.44~42.92、10.02~246.09、2.51~47.37μg·g^-1。结论：所建立的红禾麻LC-ESI-MS含量测定方法快速灵敏，准确可靠，可用于红禾麻质量控制。  

Objective: To establish an UPLC-ESI-MS method for simultaneous determination of gallocatechin, neochlorogenic acid, epigallocatechin, catechin, chlorogenic acid, cryptochlorogenic acid, epicatechin, rutin, isoquercitrin, kaempferol-3-O-rutinoside and quercitrin in Laportea bulbifera of Miao medicine by UPLC-ESIMS. Methods: The chromatographic separation was performed on a ACQUITY UPLC BEH C₁₈ (2.1 mm×100 mm, 1.7 μm)with a mobile phase consisting of 0.1% formic acid acetonitrile-0.1% formic acid at the flow rate of 0.25 mL·min^-1. The column temperature was 45℃. Electrospray ionization source (ESI)was used combined with selected ion monitoring (SIM)mode mass spectral acquisition. Results: The linear ranges for gallocatechin, neochlorogenic acid, epigallocatechin, catechin, chlorogenic acid, cryptochlorogenic acid, epicatechin, rutin, isoquercitrin, kaempferol-3-O-rutinoside and quercitrin were 0.051-3.256, 0.050-3.200, 0.056-3.594, 0.050-3.206, 0.109-6.975, 0.053-3.394, 0.012-3.087, 0.012-50.800, 0.026-3.363, 0.065-26.550 and 0.013-3.328 mg·L^-1 showed good respectively (r²>0.999), whose average recoveries were 94%-103%. The contents of gallocatechin, neochlorogenic acid, epigallocatechin, catechin, chlorogenic acid, cryptochlorogenic acid, epicatechin, rutin, isoquercitrin, kaempferol-3-O-rutinoside and quercitrin in 13 bantches of Laportea bulbifera of Miao medicine were 2.00-27.45, 2.41-20.76, 1.63-27.57, 1.75-20.80, 16.35-115.81, 4.28-20.04, 0.48-17.41, 102.90-935.53, 9.44-42.92, 10.02-246.09 and 2.51-47.37 μg·g^-1, respectively. Conclusion: The established UPLC-ESI-MS method for determining the content of Laportea bulbifera of Miao medicine is quick, sensitive, accurate and reliable, it can be used for the quality control of Laportea bulbifera of Miao medicine. 

[1] 贵州省药品监督管理局.贵州省中药材、民族药材质量标准[S].贵阳:贵州科学技术出版社, 2003:187 Drug Administration of Guizhou Province. Quality Standard of Chinese Herbal Medicine and National Medicine in Guizhou[S]. Guiyang:Guizhou Science and Technology Publishing House,2003:187
[2] 国家中医药管理局《中华本草》编委会.中华本草·苗药卷[M].贵阳:贵州科学技术出版社,2005:283 Editorial Committee of China National Materia Medica Administration. Chinese Materia Medica·Miao Medicine Roll[M]. Guiyang:Guizhou Science and Technology Publishing House,2005:283
[3] 孙庆文,徐文芬,齐维娜,等.苗药红禾麻与易混品艾麻的生药鉴别研究[J].中药材,2015, 38(9):1862 SUN QW, XU WF, QI WN, et al. To study the crude drug identification of Laportea bulbifera of Miao medicine and easymixed Laportea cuspidate[J]. J Chin Med Mater, 2015, 38(9):1862
[4] 汪石丽.红禾麻抗炎镇痛物质基础及质量控制研究[D].贵阳:贵阳医学院, 2015 WANG SL. Material Basis for the Anti-Infla Mmatory and Analgesic Effects of Laportea bulbifera and its Quality Control[D]. Guiyang:Guiyang Medical College,2015
[5] 汪石丽,李勇军,廖尚高,等. HPLC同时测定黔产红禾麻中4种儿茶素类成分含量[J].中国实验方剂学杂志, 2014, 20(21):91 WANG SL, LI YJ, LIAO SG, et al. Simultaneous determination of four catechins in Laportea bulbifera by HPLC[J]. Chin J Exp Tradit Med Form,2014, 20(21):91
[6] 苏志强,赵增宇,谢胜男,等.红活麻提取物镇痛抗炎和免疫抑制活性研究[J].中国药理学通报, 2009, 25(4):559 SUN ZQ, ZHAO ZY, XIE SN, et al. Effect of analgesia, antiinfla mmation and immunosuppression of acetic ether extract of Chinese medicine Honghuoma[J]. Chin Pharmacol Bull, 2009, 25(4):559
[7] 马琳,梁冰,朱珠,等.民族药珠芽艾麻醇提物镇痛药理作用的研究[J].贵阳中医学院学报,2012, 34(1):24 MA L, LIANG B, ZHU Z, et al. To research the analgesia pharmacologica action of the ethanolic extrat of national medicine Laportea bulbifeara[J]. J Guiyang Coll Tradit Chin Med, 2012, 34(1):24
[8] 唐娟,吴耽,陈思颖,等.基于UPLC-ESI-Q-TOF-MS的红禾麻提取物化学成分分析[J].中国实验方剂学杂志, 2018,(10):1 TANG J, WU D, CHEN SY, et al. Identification of chemical compositions in Laportea bulbifera by UPLC-ESI-Q-TOF-MS[J]. Chin J Exp Tradit Med Form,2018, 24(10):1
[9] 孙大赢,赵文法,李广华,等. LC-MS/MS法同时测定参芍胶囊中人参皂苷和芍药苷的含量[J].药物分析杂志, 2018, 38(1):186 SUN DY, ZHAO WF, LI GH, et al. Simultaneous determination of ginsenosides and paeoniflorin in Shenshao capsules by LC-MS/MS[J]. Chin J Pharm Anal,2018, 38(1):186
[10] 唐蕾,王琳玲,徐新元.液相色谱-质谱联用同时测定芪胶升白胶囊中黄芪甲苷、淫羊藿苷、阿魏酸的含量[J].药物分析杂志, 2016, 36(12):2199 TANG L, WANG LL, XU XY. Simultaneous determination of the contents of astragaloside IV, icariin and ferulic acid in Shenbai capsules by LC-MS[J]. Chin J Pharm Anal,2016, 36(12):2199
[11] 宋凡,宋晓妮,王磊,等.酒石酸伐尼克兰中6个类苯胺基因毒性杂质的LC-MS法测定[J].药物分析杂志, 2018, 38(1):130 SONG F,SONG XN,WANG L,et al. Determination of six anilinelike genotoxic impurities in varenicline tartrate by LC-MS[J]. Chin J Pharm Anal,2018, 38(1):130
[12] 梁琨,孙辉,安叡,等. LC-MS/MS法同时测定护心口服液中11种成分[J].中成药,2018, 40(1):105 LIANG K, SUN H, AN R, et al. Simultaneous determination of eleven constituents in Huxin oral liquid by LC-MS/MS[J]. Chin Tradit Pat Med,2018, 40(1):105
[13] 潘立卫,罗泽萍,范明燕. HPLC法同时测定华山矾中8种成分的含量[J].中药材,2017, 40(6):1377 PAN LW, LUO ZP, FAN MY. Simultaneous determination of eight constituents in Symplocos chinensis by HPLC[J]. J Chin Med Mater, 2017, 40(6):1377
[14] 胡莹,吴啟南,郑啸,等. LC-MS/MS法同时测定金樱子中7种主要成分的含量[J].中药材,2016, 39(12):2798 HU Y, WU QN, ZHEN X, et al. Simultaneous determination of seven constituents in Rosa laevigata Michx. by LC-MS/MS[J]. J Chin Med Mater, 2016, 39(12):2798
[15] 杨才琼,吴海军,张潇文,等. LC-MS测定黑豆中异黄酮和花色苷的含量[J].天然产物研究与开发, 2018, 30(5):817 YANG CQ, WU HJ,ZHANG XW,et al. Determination of isoflavone and anthocyanin in black soybean seed(Glycine max)by LC-MS[J]. Nat Prod Res Dev,2018, 30(5):817