目的:建立UPLC-MS/MS 方法同时测定养胃汤中26个成分(厚朴酚、和厚朴酚、木兰花碱、木兰箭毒碱、木兰苷A、木兰苷B、橙皮苷、川陈皮素、橘皮素、甜橙黄酮、芸香柚皮苷、柚皮素、人参皂苷Rb1、6-姜辣素、甘草苷、甘草酸、甘草素、异甘草素、异甘草苷、芹糖异甘草苷、毛蕊花糖苷、异毛蕊花糖苷、绿原酸、新绿原酸、咖啡酸、芦丁)的含量。方法:采用Shim-pack GIST C18色谱柱(2.1 mm×100 mm,2.0 μm),以乙腈-0.1%乙酸-1 mmol·L-1乙酸铵水为流动相,进行梯度洗脱,柱温为30 ℃,流速为0.3 mL·min-1,进样量为1 μL,分析时间为18 min。采用电喷雾电离源(ESI源),以多重反应监测(MRM)模式正负离子检测。结果:所测26个化学成分在测定浓度范围内线性关系良好,相关系数均大于0.996 9;精密度、重复性和稳定性良好;平均加样回收率为96.5%～104.2%,RSD≤4.0%。6批样品中厚朴酚、和厚朴酚、木兰花碱、木兰箭毒碱、木兰苷A、木兰苷B、橙皮苷、川陈皮素、橘皮素、甜橙黄酮、芸香柚皮苷、柚皮素、人参皂苷Rb1、6-姜辣素、甘草苷、甘草酸、甘草素、异甘草素、异甘草苷、芹糖异甘草苷、毛蕊花糖苷、异毛蕊花糖苷、绿原酸、新绿原酸、咖啡酸、芦丁的含量测定结果分别为2 814.12~2 951.41、2 551.48~2 675.66、288.12~312.36、439.88~494.60、452.00~500.74、329.76~358.68、5 995.57~6 283.13、70.16~73.81、22.95~24.21、5.56~6.39、997.32~1 077.03、6.17~6.81、643.88~674.16、994.16~1 063.20、1 929.00~1 984.85、2 356.80~2 518.96、247.68~256.64、38.02~43.18、228.84~241.4、227.17~234.87、129.61~150.39、28.97~31.90、622.85~643.23、526.05~542.73、70.09~78.64、152.41~166.3 μg·g-1。结论:本方法准确灵敏,稳定性和重复性好,可用于养胃汤的质量控制。
Objective: To establish an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous determination of twenty six components(magnolol, honokiol, magnolflorine, magnocurarine, magnoloside A, magnoloside B, hesperidin, nobiletin, tangeretin, sinensetin, narirutin, naringenin, ginsenoside Rb1, 6-gingerol, liquiritin, glycyrrhizic acid, liquiritigenin, isoliquiritigenin, isoliquiritin, isoliquiritin apioside, verbascoside, isoacteoside, chlorogenic acid, neochlorogenic acid, caffeic acid and rutin)in Yangwei decoction. Methods: The separation was performed on a Shim-pack GIST C18 column (2.1 mm×100 mm,2.0 μm) with a mobile phase consisting of acetonitrile and 0.1% acetic acid-1 mmol·L-1 ammonium acetate water solution with gradient elution at a flow rate of 0.3 mL·min-1. The column temperature was 30 ℃, the injection volume was 1 μL and the analysis time was 18.0 min. The detection was carried out by electrospray ionization (ESI). Positive and negative electrospray ionization was performed in multiple reaction monitoring (MRM) mode. Results: All of the analytes showed good linearity (r≥0.996 9) in the tested ranges. The precision, repeatability and stability of the method were good for the twenty six components. The average recoveries were in the range of 96.5%~104.2% with relative standard deviations RSD≤4.0%. The contents of magnolol, honokiol, magnolflorine, magnocurarine, magnoloside A, magnoloside B, hesperidin, nobiletin, tangeretin, sinensetin, narirutin, naringenin, ginsenoside Rb1, 6-gingerol, liquiritin, glycyrrhizic acid, liquiritigenin, isoliquiritigenin, isoliquiritin, isoliquiritin apioside, verbascoside, isoacteoside, chlorogenic acid, neochlorogenic acid, caffeic acid and rutin in 6 batches of Yangwei decoction were 2 814.12-2 951.41, 2 551.48-2 675.66, 288.12-312.36, 439.88-494.60, 452.00-500.74, 329.76-358.68, 5 995.57-6 283.13, 70.16-73.81, 22.95-24.21, 5.56-6.39, 997.32-1 077.03, 6.17-6.81, 643.88-674.16, 994.16-1 063.20, 1 929.00-1 984.85, 2 356.80-2 518.96, 247.68-256.64, 38.02-43.18, 228.84-241.4, 227.17-234.87, 129.61-150.39, 28.97-31.90, 622.85-643.23, 526.05-542.73, 70.09-78.64 and 152.41-166.3 μg·g-1, respectively. Conclusion: The established method is accurate, stable and reproducible,and can provide a research method for the quality control of Yangwei decoction.
[1] 关于发布《古代经典名方目录(第一批)》的通知[EB/OL]. 国家中医药管理局, 2018[2018-04-13]. http://kjs.satcm.gov.cn/zhengcewenjian/2018-04-16/7107.html
Notice on the issuance of the《Catalog of Ancient Classical Prescriptions (First Batch)》[EB/OL]. State Administration of Traditional Chinese Medicine, 2018[2018-4-13]. http://kjs.satcm.gov.cn/zhengcewenjian/2018-04-16/7107.html
[2] LUO H, WU H, YU X, et al. A review of the phytochemistry and pharmacological activities of Magnoliae officinalis cortex[J].J Ethnopharmacol, 2019, 236: 412
[3] GUO K, TONG C, FU Q, et al. Identification of minor lignans, alkaloids, and phenylpropanoid glycosides in Magnolia officinalis by HPLC-DAD-QTOF-MS/MS[J].J Pharm Biomed Anal 2019, 170: 153
[4] YU X, SUN S, GUO Y, et al. Citri Reticulatae Pericarpium (Chenpi): botany, ethnopharmacology, phytochemistry, and pharmacology of a frequently used traditional Chinese medicine[J].J Ethnopharmacol, 2018, 220: 265
[5] ZHAO LH, ZHAO HZ, ZHAO X, et al. Simultaneous quantification of seven bioactive flavonoids in Citri Reticulatae Pericarpium by ultra fast liquid chromatography coupled with tandem mass spectrometry[J].Phytochem Anal, 2016, 27(3): 168
[6] SWAMY MK, SINNIAH, UR. A comprehensive review on the phytochemical constituents and pharmacological activities of Pogostemon cablin Benth.: an aromatic medicinal plant of industrial importance[J].Molecules, 2015, 20(5): 8521
[7] WANG YZ, ZHANG J, ZHAO YL, et al. Mycology, cultivation, traditional uses, phytochemistry and pharmacology of Wolfiporia cocos (Schwein.) Ryvarden et Gilb.: a review[J].J Ethnopharmacol, 2013, 147(2): 265
[8] 张博, 孙秀丽, 郭云龙, 等. 液质联用技术分析不同产地不同年限人参的化学成分[J].中国实验方剂学杂志, 2020, 26(8): 206
ZHANG B, SUN XL, GUO YL, et al. Chemical constituents of ginseng radix et Rhizoma with different growth years and different origins based on LC-MS[J].Chin J Exp Tradit Med Form, 2020, 26(8): 206
[9] JIANG M, ZHAO S, YANG S, et al. An "essential herbal medicine"-licorice: a review of phytochemicals and its effects in combination preparations[J].J Ethnopharmacol, 2020, 249: 112439
[10] 杨阳, 辛杨, 马凤延, 等. UHPLC-Q-Exactive-Obitriap MS快速定量附子理中汤10种化学成分[J].中草药, 2020, 51(7): 1839
YANG Y, XIN Y, MA FY, et al. UHPLC-Q-Exactive-Obitriap MS for quantification of ten components in Fuzi Lizhong Decoction[J].Chin Tradit Herb Drugs, 2020, 51(7): 1839
[11] 朱鹤云, 王开鼎, 史健艺, 等. UFLC-MS/MS法同时测定栀子厚朴汤中10个成分的含量[J].药物分析杂志, 2020, 40(10): 1751
ZHU HY, WANG KD, SHI JY, et al. Simultaneous determination of ten components in Zhizi Houpo decoction by UFLC-MS/MS[J].Chin J Pharm Anal, 2020, 40(10): 1751
[12] 张诚贤, 吴芳媛, 陈褚建, 等. 超高效液相色谱-串联质谱法同时测定木香顺气丸中10个成分的含量[J].药物分析杂志, 2021, 41(6): 1064
ZHANG CX, WU FY, CHEN CJ, et al. Simultaneous determination of ten components in Muxiang Shunqi pills by UPLC-MS/MS[J].Chin J Pharm Anal, 2021, 41(6): 1064
[13] 董乙文, 李天雪, 褚朝森, 等. UPLC-MS/MS法同时定量测定补中益气丸中的15种化合物[J].药物分析杂志, 2017, 37(7): 1228
DONG YW, LI TX, CHU CS, et al. UPLC-MS/MS method for simultaneous determination of 15 components in Buzhong Yiqi pills[J].Chin J Pharm Anal, 2017, 37(7): 1228
[14] ZHU MZ, CHEN GL, WU JL, et al. Recent development in mass spectrometry and its hyphenated techniques for the analysis of medicinal plants[J].Phytochem Anal, 2018, 29(4): 365
[15] 吴蓓, 李军茂, 黄小方, 等. UHPLC-MS/MS法同时测定杏香兔耳风中13种成分的含量[J].中草药, 2020, 51(15): 4025
WU B, LI JM, HUANG XF, et al. Simultaneous determination of thirteen components in Ainsliaea fragrans by UHPLC-MS/MS[J].Chin Tradit Herb Drugs, 2020, 51(15): 4025
[16] 魏欣, 杨金霞, 孙雅晴, 等. UPLC-MS/MS法同时测定木蝴蝶中10个有效成分[J].中草药, 2020, 51(8):2221
WEI X, YANG JX, SUN YQ, et al. Simultaneous determination of ten components in Oroxylum indicum by UPLC-MS/MS[J].Chin Tradit Herb Drugs, 2020, 51(8): 2221
[17] 傅春燕, 王惠余, 刘永辉, 等. 基于UPLC-ESI-IT-TOF-MS方法对血府逐瘀汤中8个成分同时含量测定[J].天然产物研究与开发, 2020, 32(6): 1006
FU CY, WANG HY, LIU YH, et al. Simultaneous determination of eight components in Xuefu Zhuyu decoction based on UPLC-ESI-IT-TOF-MS method[J].Nat Prod Res Dev, 2020, 32(6): 1006
[18] 周佳, 蔡皓, 段煜, 等. 基于UHPLC-QqQ-MS的四逆散水提液中16种主要化学成分的定量研究[J].南京中医药大学学报, 2019, 35(1): 85
ZHOU J, CAI H, DUAN Y, et al. Simultaneous determination of 16 main chemical componets in aqueous extract of Sinisan based on UHPLC-QqQ-MS technology[J].J Nanjing Univ Tradit Chin Med, 2019, 35(1): 85
