HPLC-MS/MS法同时测定蒙药森登-4颗粒剂中15种成分的含量  

Simultaneous determination of 15 constituents in Sendeng-4 Granules of Mongolian medicine by HPLC-MS/MS

作　　者：李君[1,2,3] 常福厚 白图雅 胡玉霞[1,2,3] 张梦迪 周树宏[1,2,4] LI Jun;CHANG Fuhou;BAI Tuya;HU Yuxaia;ZHANG Mengdi;ZHOU Shuhong(The Center for New Drug Safety Evaluation and Research,Inner Mongolia Medical University,Hohhot O10110,China;Research Center for Drug Screening,Inner Mongolia Autonomous Region,Hohhot 010110,China;College of Pharmacy,Inner Mongolia Medical University,Hohhot 010110,China;School of Basic Medicine,Inner Mongolia Medical University,Hohhot O10110,China)

机构地区：[1]内蒙古医科大学新药安全评价研究中心,内蒙古呼和浩特010110 [2]内蒙古自治区新药筛选工程研究中心,内蒙古呼和浩特010110 [3]内蒙古医科大学药学院,内蒙古呼和浩特010110 [4]内蒙古医科大学基础医学院,内蒙古呼和浩特010110

出　　处：《沈阳药科大学学报》2023年第5期601-612,共12页Journal of Shenyang Pharmaceutical University

基　　金：国家自然科学基金资助项目(81760676);内蒙古自治区自然科学基金(2022LHQN08001);内蒙古自治区卫生健康委医疗卫生科技计划项目(202201186);内蒙古自治区高等学校科学研究项目(NJZY22655);内蒙古医科大学面上项目(YKD2022MS038)。

摘　　要：目的建立HPLC-MS/MS法同时测定蒙药森登-4颗粒中15种成分(鞣花酸、没食子酸、柯里拉京、西红花苷Ⅰ、栀子苷、阿魏酸、槲皮素、川楝素、芦丁、绿原酸、木犀草素、儿茶素、表儿茶素、杨梅素、二氢杨梅素)的含量。方法采用HPLC-MS/MS法分析,色谱柱为Shim-pack GIST-HP C_(18)(100 mm×2.1 mm,3μm)柱;流动相为甲醇(A)-体积分数0.1%甲酸水溶液(B),梯度洗脱;流速为0.25 mL·min^(-1),进样量为3μL,柱温为35℃;质谱条件:采用电喷雾电离源,负离子模式扫描,多反应监测模式检测各成分。结果森登-4颗粒中鞣花酸、没食子酸、柯里拉京、西红花苷Ⅰ、栀子苷、阿魏酸、槲皮素、川楝素、芦丁、绿原酸、木犀草素、儿茶素、表儿茶素、杨梅素、二氢杨梅素分别在质量浓度为273.50~13675.00μg·L^(-1)、21.80~1090.00μg·L^(-1)、63.60~3180.00μg·L^(-1)、25.55~1277.50μg·L^(-1)、45.80~2290.00μg·L^(-1)、2.55~1275.00μg·L^(-1)、5.66~283.00μg·L^(-1)、4.50~225.00μg·L^(-1)、4.64~232.00μg·L^(-1)、5.70~285.00μg·L^(-1)、0.126~6.30μg·L^(-1)、24.70~1235.00μg·L^(-1)、56.40~2820.00μg·L^(-1)、25.4~1270.00μg·L^(-1)、49.2~2460.00μg·L^(-1)内具有良好的线性关系(r≥0.9991);平均加样回收率为93.77%~109.17%(RSD<2%)。6批次森登-4颗粒样品中上述15种成分的含量范围分别为12.353~14.742 mg·g^(-1)、2.635~2.921 mg·g^(-1)、13.711~15.495 mg·g^(-1)、4.112~4.884 mg·g^(-1)、25.573~28.284 mg·g^(-1)、0.036~0.042 mg·g^(-1)、0.400~0.469 mg·g^(-1)、0.711~0.803 mg·g^(-1)、0.592~0.668 mg·g^(-1)、0.187~0.211 mg·g^(-1)、3.558~3.875μg·g^(-1)、2.117~2.358 mg·g^(-1)、14.018~15.845 mg·g^(-1)、3.918~4.961 mg·g^(-1)、16.885~18.659 mg·g^(-1)。结论所建立的HPLC-MS/MS含量测定方法可用于蒙药森登-4颗粒的质量控制。Objective To establish an HPLC-MS/MS method for simultaneous determination of 15 chemical constituents(ellagic acid, gallic acid, corilagin, crocetin Ⅰ,geniposide, ferulic acid, quercetin, chuanmusu, rutin, chlorogenic acid, luteolin, catechin, epicatechin, myricetin and dihydromyricetin)in Sendeng-4 Granules(SD-4).Methods The HPLC-MS/MS method was used and the chromatographic conditions were as follows: the column was Shim-pack GIST-HP C_(18)(100 mm×2.1 mm, 3 μm),the mobile phase was consisted of methanol-water(containing 0.1%formic acid)at a flow rate of 0.25 mL·min^(-1) with gradient elution.The injection volume was 3 μL,and the column temperature was 35 ℃.Mass spectrometer conditions: a triple quadrupole mass spectrometer equipped with electrospray ionization source(ESI)was used in negative ion mode using multiple reaction monitoring(MRM).Results Under the optimized conditions, ellagic acid, gallic acid, corilagin, crocetin Ⅰ,geniposide, ferulic acid, quercetin, chuanmusu, rutin, chlorogenic acid, luteolin, catechin, epicatechin, myricetin and dihydromyricetin all showed good liners in the range of 273.50-13 675.00 μg·L^(-1),21.80-1 090.00 μg·L^(-1),63.60-3 180.00 μg·L^(-1),25.55-1 277.50 μg·L^(-1),45.80-2 290.00 μg·L^(-1),2.55-1 275.00 μg·L^(-1),5.66-283.00 μg·L^(-1),4.50-225.00 μg·L^(-1),4.64-232.00 μg·L^(-1),5.70-285.00 μg·L^(-1),0.126-6.30 μg·L^(-1),24.70-1 235.00 μg·L^(-1),56.40-2820.00 μg·L^(-1),25.4-1 270.00 μg·L^(-1) and 49.2-2 460.00 μg·L^(-1),respectively.The recoveries were ranged from 93.77%-109.17%with RSD≤2%.And the average contents of 15 active components in 6 batches of SD-4 granules were 12.353-14.742 mg·g^(-1),2.635-2.921 mg·g^(-1),13.711-15.495 mg·g^(-1),4.112-4.884 mg·g^(-1),25.573-28.284 mg·g^(-1),0.036-0.042 mg·g^(-1),0.400-0.469 mg·g^(-1),0.711-0.803 mg·g^(-1),0.592-0.668 mg·g^(-1),0.187-0.211 mg·g^(-1),3.558-3.875 μg·g^(-1),2.117-2.358 mg·g^(-1),14.018-15.845 mg·g^(-1),3.918-4.961 mg·g^(-1) and 16.885-18.659 mg·g^(-1).Conclusion

关 键 词：森登-4颗粒 高效液相色谱串联三重四级杆质谱 多组分含量测定 质量控制 

分 类 号：R917[医药卫生—药物分析学]