目的: 建立超高效液相色谱 - 串联质谱法（UPLC-MS/MS）同时测定木香顺气丸中木香烃内酯、 去氢木香内酯、和厚朴酚、厚朴酚、甘草酸、甘草苷、橙皮苷、柚皮苷、新橙皮苷、辛弗林 10 个成分的含量。方法: 采用 Waters ACQUITY UPLC BEH C18 色谱柱（2.1 mm×100 mm,1.7 µm）,流动相为 0.1% 甲酸乙腈 溶液 -0.1% 甲酸水溶液,梯度洗脱,流速为 0.3 mL·min-1,柱温为 35 ℃,采用电喷雾离子源（ESI）,正负离 子同时扫描,多反应监测模式（MRM）对 10 个成分进行检测。结果: 10 个成分在测定的质量浓度范围内 线性关系良好,相关系数（r）均大于 0.995,平均回收率为 92.8%~106.8%,RSD 为 1.6%~4.6%。6 批木香顺气丸中木香烃内酯、去氢木香内酯、和厚朴酚、厚朴酚、甘草酸、甘草苷、橙皮苷、柚皮苷、新橙皮苷和辛 弗林的含量范围分别为 0.467~0.923、1.276~2.127、0.748~4.665、2.081~4.791、0.887~1.012、0.234~0.422、14.892~23.516、3.539~6.799、2.652~5.072 和 0.259~0.570 mg·g-1。结论: 所建立的方法快速、准确,适用于木香顺气丸中木香烃内酯、去氢木香内酯、和厚朴酚、厚朴酚、甘草酸、甘草苷、橙皮苷、柚皮苷、新橙皮苷和 辛弗林 10 个成分的含量测定,为木香顺气丸多组分质量控制提供参考。
Objective: To establish an ultra-performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）method for simultaneous determination of costunolide,dehydrocostus lactone,honokiol, magnolol,glycyrrhizic acid,liquiritin,hesperidin,naringin,neohesperidin and synephrine in Muxiang Shunqi pills. Methods: The components were separated on Waters ACQUITY UPLC BEH C18 column（2.1 mm×100 mm,1.7 µm）with 0.1% formic acid acetonitrile solution and 0.1% formic acid aqueous solution as the mobile phase by gradient elution. The flow rate was 0.3 mL·min-1. The column temperature was set at 35 ℃. The detection was carried out by electrospray ionization（ESI）in positive and negative modes. Multiple reaction monitoring （MRM）mode was used for quantitative analysis. Results: The linear relationships of ten components were good in corresponding concentrations with correlation coefficients（r）grenter 0.995. The average recoveries of ten components were 92.8%-106.8% with RSDs within 1.6%-4.6%. The contents of costunolide,dehydrocostus lactone,honokiol,magnolol,glycyrrhizic acid,liquiritin,hesperidin,naringin,neohesperidin and synephrine in Muxiang Shunqi pills were 0.467-0.923,1.276-2.127,0.748-4.665,2.081-4.791,0.887-1.012,0.234-0.422, 14.892-23.516,3.539-6.799,2.652-5.072 and 0.259-0.570 mg·g-1,respectively. Conclusion: The method is rapid,accurate and suitable for simultaneous determination of costunolide,dehydrocostus lactone,honokiol, magnolol,glycyrrhizic acid,liquiritin,hesperidin,naringin,neohesperidin and synephrine in Muxiang Shunqi pills. The method can provide reference for the quality control of Muxiang Shunqi pills.
[1] 中华人民共和国药典 2020 年版.一部[S].2020:639 ChP 2020.Vol Ⅰ[S].2020:639
[2] 赖增发,夏丽珍.“一测多评”测定木香顺气丸中木香内酯类成分[J].中国现代应用药学,2014,31(4):421
LAI ZF,XIA LZ.Determination of costuslactone in Muxiang Shunqi pills by QAMS[J].Chin J Mod Appl Pharm,2014,31(4):421
[3] 师健友,童荣生,李晋奇,等.HPLC 测定木香顺气丸中的木香烃内酯[J].华西药学杂志,2013,28(4):417
SHI JY,TONG RS,LI JQ,et al.Determination of costunolide in Muxiang Shunqi pills by HPLC[J].West China J Pharm Sci,2013, 28(4):417
[4] 姜宁,刘晓鹏,高秀丽,等.快速提取及测定木香顺气丸中厚朴酚与和厚朴酚的研究[J].江西师范大学学报(自然科学版), 2007,31(4):347
JIANG N,LIU XP,GAO XL,et al.A study on the extracting and determining method for magnolol and honokiol in Muxiang Shunqi pills[J].J Jiangxi Norm Univ(Nat Sci),2007,31(4):347
[5] 曹瑞竹. 木香顺气丸 HPLC 特征指纹图谱研究及多成分含量测定[J].药物分析杂志,2017,37(6):1127
CAO RZ.Fingerprint and multi-components determination of Muxiang Shunqi pills by HPLC[J].Chin J Pharm Anal,2017,37(6):1127
[6] 万慧杰,王建国,朱贺年.RP-HPLC 测定木香顺气丸中橙皮苷的含量[J].中国实验方剂学杂志,2010,16(16):67
WAN HJ,WANG JG,ZHU HN.HPLC determination of hesperidin in Muxiang Shunqi pills[J].Chin J Exp Tradit Med Form,2010,16(16):67
[7] 张运杰,彭朝霞,熊然英,等.HPLC 测定木香顺气丸中橙皮苷的含量[J].中国现代中药,2007,9(6):20
ZHANG YJ,PENG ZX,XIONG RY,et al.Determination of hesperidin in Muxiang Shunqi pills by HPLC[J].Mod Chin Med, 2007,9(6):20
[8] 徐成志. HPLC 法测定木香顺气丸中橙皮苷的含量[J].安徽医药,2007,11(1):36
XU CZ.Determination of hesperidin in Muxiang Shunqi pills by HPLC[J].Anhui Med Pharm J,2007,11(1):36
[9] 王嘉林. 亲水作用色谱测定木香顺气丸中辛弗林的含量[J].中国药事,2014,28(12):1361
WANG JL.Determination the epinephrine in Muxiang Shunqi pills with HILIC Chromatography[J].Chin Pharm Aff,2014,28(12): 1361
[10] 陈洁. UPLC-MS/MS 法同时测定香青兰中 6 个活性成分的含量[J].药物分析杂志,2020,40(11):1986
CHEN J.Simultaneous determination of 6 active ingredients in Dracocephalum moldavica L.by UPLC-MS/MS[J].Chin J Pharm Anal,2020,40(11):1986
[11] 张迪文,马开,田萍.UPLC-MS/MS 法同时测定金花葵中 11 个活性成分[J].药物分析杂志,2019,39(5):780
ZHANG DW,MA K,TIAN P.Simultaneous determination of 11 active components in Aurea helianthus by UPLC-MS/MS[J].Chin J Pharm Anal,2019,39(5):780
[12] 刘蓬蓬,单国顺,张凡,等.UPLC-MS 比较有机酸定向炮制黄芪中12 种活性成分的含量[J].中国中药杂志,2020,45(1):113
LIU PP,SHAN GS,ZHANG F,et al.Comparison of 12 constituents of Astragali Radix directionally processed with organic acid by UPLC-MS[J].China J Chin Mater Med,2020,45(1):113
[13] 张艳丽,杨雁芸,白志尧,等.UPLC-MS/MS 同时测定熟地黄中 8 个核苷类成分的含量[J].药物分析杂志,2019,39(4):608 ZHANG YL,YANG YY,BAI ZY,et al.Simultaneous determination of eight nucleosides in Rehmanniae Radix Praeparata by UPLC-MS/MS[J].Chin J Pharm Anal,2019,39(4):608
[14] 覃华亮,覃子龙,符传武,等.UPLC-MS/MS 多组分快速测定结合化学模式识别的玉叶清火片质量控制研究[J].中草药,2019, 50(22):5470
QIN HL,QIN ZL,FU CW,et al.Quality control research of Yuye Qinghuo tablets by UPLC MS/MS multicomponent determination coupled with chemical pattern recognition[J].Chin Tradit Herb Drugs,2019,50(22):5470
[15] 支旭然,王觅,宋浩静,等.UPLC-MS/MS 法同时测定舒肝宁注射液中 6 个成分的含量[J].药物分析杂志,2018,38(12):2194
ZHI XR,WANG M,SONG HJ,et al.Simultaneous determination of 6 components in Shuganning injection by UPLC-MS/MS[J].Chin J Pharm Anal,2018,38(12):2194
[16] 夏鸿林,胡翔.UPLC-MS/MS 法同时定量分析暖宫孕子胶囊中的10 个成分[J].药物分析杂志,2018,38(7):1158
XIA HL,HU X.Simultaneous determination of ten components in Nuangong Yunzi capsules by UPLC-MS/MS[J].Chin J Pharm Anal,2018,38(7):1158
