目的:建立UPLC-MS/MS法同时测定排石合剂中京尼平苷酸、羟基红花黄色素A、绿原酸、苦杏仁苷、王不留行黄酮苷、甘草苷、毛蕊花糖苷、杯苋甾酮、丹皮酚、甘草酸铵10个特征成分的含量。方法:供试品经70%甲醇超声处理,Waters HSS T3 C18(100 mm×2.1 mm,1.7 μm)色谱柱,以乙腈-0.1%甲酸为流动相进行梯度洗脱,流速0.3 mL·min-1;电喷雾正负离子源同时监测,多反应监测(MRM)模式。结果:方法重复性、准确度良好,10个成分的平均回收率在99.0%~101.0%,RSD为0.090%~4.3%,在各自浓度范围内线性关系良好,含量结果分别为31.129~34.256、95.456~98.741、126.85~129.43、238.62~240.90、45.620~47.520、26.124~28.412、13.852~15.030、16.632~17.854、800.41~805.56、78.485~80.963 μg·mL-1。结论:本研究建立的方法快速简便,选择性好,准确可靠,为排石合剂的质量控制提供科学依据。
Objective:To establish simultaneous determination method of 10 representative components in Paishi mixture, including geniposidic acid, hydroxyl-safflor yellow A, chlorogenic acid, amygdalin, vaccarin, liquiritin, mulberry glycoside, cyclamenone, paeonol and ammonium glycyrrhizinate. Methods: The sample was ultrasonicated with 70% methanol. The chromatographic separation was performed on a Waters HSS T3 C18(100 mm×2.1 mm,1.7 μm)column with acetonitrile-0.1% formic acid solution as mobile phase with gradient elution. The flow rate was 0.3 mL·min-1. The analytes were detected by tandem mass spectrometry under the positive and negative ion modes with the ESI source and multiple reaction monitoring (MRM) mode. Results: The repeatability and accuracy of the method were good, and the average recoveries were 99.0%-101.0% with RSDs of 0.090%-4.3%. The sample determination results showed that there were differences in the consistency between batches of preparations. The contents of 10 components were 31.129-34.256, 95.456-98.741, 126.85-129.43, 238.62-240.90, 45.620-47.520, 26.124-28.412, 13.852-15.030, 16.632-17.854, 800.41-805.56, 78.485-80.963 μg·mL-1. Conclusion: The developed method is simple, rapid and accurate, which provides a more comprehensive scientific basis for the quality evaluation of Kechuan mixture.
[1] 中华人民共和国药典2020年版. 一部[S]. 2020: 229
ChP 2020. Vol Ⅰ[S]. 2020: 229
[2] 张恒斌, 王亮. UPLC-Q-Orbitrap高分辨质谱定量分析风寒感冒颗粒中的11个成分[J].药物分析杂志, 2019, 39(10):1828
ZHANG HB, WANG L. Simultaneous determination of 11 components in Fenghan Ganmao granules by UPLC-Q-Orbitrap high-resolution mass spectrometry[J]. Chin J Pharm Anal, 2019, 39(10):1828
[3] 杨洋, 杨光义, 张子龙, 等. 超高效液相色清法测定麻黄宣肺止咳糖浆中7种有效成分含量[J]. 时珍国医国药, 2019, 30(4):820
YANG Y, YANG GY, ZHANG ZL, et al. Determination of 7 active ingredients in Mahuang Xuanfei Zhike syrup by ultra performance liquid chromatography[J]. Lishizhen Med Mater Med Res, 2019, 30(4):820
[4] 康俊丽, 黄海英, 刘雅敏, 等. 基于UPLC-QE-Orbitrap-MS法测定补肺益肾方中10个入血成分的含量[J]. 药物分析杂志, 2019, 39(3):441
KANG JL, HUANG HY, LIU YM, et al. Simultaneous determination of 10 absorbed active components in rat plasma of BUfei Yishen recipe by UPLC-QE-Qrbitrap-MS[J]. Chin J Pharm Anal, 2019, 39(3):441
[5] 陈明曦, 李艳梅, 孙婷, 等. 液相色谱-质谱联用技术在中药质量研究中的应用[J]. 中国药剂学杂志, 2021, 19(1):12
CHEN MX, LI YM, SUN T, et al. Application of liquid chromatography/mass spectrometry in quality research of traditional Chinese medicine[J]. Chin J Pharm, 2021, 19(1):12
[6] 黄砚, 刁灏瑒, 张雁. 克咳片中8个成分的含量测定[J]. 药物分析杂志, 2020, 40(2):337
HUANG Y, DIAO HY, ZHANG Y. Determination of 8 constituents in Keke tablets[J]. Chin J Pharm Anal, 2020, 40(2):377
[7] 宋兴发, 周军, 郭守城. 杏仁止咳合剂HPLC指纹图谱及7种成分的含量测定[J]. 中国现代应用药学, 2020, 37(1):50
SONG XF, ZHOU J, GUO SC. Study on HPLC fingerprints and content determination of 7 components in Xingren Zhike mixture[J]. Chin J Mod Appl Pharm, 2020, 37(1):50
[8] 张项, 蔺千, 唐玉婷. HPLC波长切换法同时测定小儿清热止咳口服液中8种成分的含量[J]. 中国药师, 2019, 22(8):1531
ZHANG X, LIN Q, TANG YT. Simultaneous determination of 8 constituents in Qingre Zhike oral liquid by HPLC wavelength switching method[J]. China Pharm, 2019, 22(8):1531
[9] 顾瑶华, 巢为农. UPLC-MS/MS测定五味消炎灵含片中5种成分的含量[J]. 南京中医药大学学报, 2014, 30(6):578
GU YH, CHAO WN. The quantitative analysis of five compounds from Wu-Wei-Xiao-Yan-Ling Buccal tablets by the ultra high performance liquid chromatography coupled with tandem mass spectrometry[J]. J Nanjing Univ Tradit Chin Med, 2014, 30(6):578
[10] 梁艳, 张峰. UPLC-MS/MS法同时测定女金胶囊中10种成分[J]. 中成药, 2021, 43(7):1713
LIANG Y, ZHANG F. Simultaneous determination of ten constituents in Nüjin cspsules by UPLC-MS/MS[J]. Chin Tradit Pat Med, 2021, 43(7):1713
[11] 何子骥, 伍斌玺, 李雨昕, 等. 基于指纹图谱和化学模式识别分析的车前子与炒车前子质量评价[J]. 中国药房, 2022, 728(14):1700
HE ZJ, WU BX, LI YX, et al. Quality evaluation of Plantago asiatica and fried Plantago asiatica based on fingerprint and analysis of chemical pattern recognition[J]. China Pharm, 2022, 728(14):1700
[12] 郑文炜, 许舒瑜, 林锦德, 等. 基于UPLC-MS/MS与G1-熵权法多指标综合评分优化净石合剂提取工艺[J]. 中国医院药学杂志, 2022, 42(24):2581
ZHENG WW, XU SY, LIN JD, et al. Optimization of extraction process of Jingshi mixture based on multi-index comprehensive evaluation of UPLC-MS/MS and G1-entropy weight method[J]. Chin Hosp Pharm J, 2022, 42(24):2581
[13] 许晓辉, 邱国玉, 景武堂, 等. 液质联用技术在新药研发中的应用[J]. 转化医学电子杂志, 2018, 5(11):90
XU XH, QIU GY, JING WT, et al. The application of liquid chromatography-mass spectrometry technology in the research and development of new drug[J]. Electron J Trans Med, 2018, 5(11):90
[14] 解笑瑜, 甄雪燕, 于航, 等. 2018年度药物分析技术研究进展[J]. 药物分析杂志, 2020, 40(5):767
XIE XY, ZHEN XY, YU H, et al. Advances in technology of pharmaceutical analysis in 2018[J]. Chin J Pharm Anal, 2020, 40(5):767
[15] 王迪, 俞佳, 詹固, 等. 液质联用技术在中药研究中的应用进展[J]. 中华中医药学刊, 2022, 40(2):68
WANG D, YU J, ZHAN G, et al. Advance in application of liquid chromatography-mass spectrometry technology in study of traditional Chinese medicine[J]. Chin Arch Tradit Chin Med, 2022, 40(2):68
