参麦颗粒中红参掺伪研究
Study on the Adulteration of Ginseng Radix et Rhizoma Rubra in Shenmai Granules
雷蓉 1刘亚茹 2王晓蕾 1刘永利1
作者信息
- 1. 河北省药品医疗器械检验研究院·河北省中药质量评价与标准研究重点实验室,河北 石家庄 050227
- 2. 河北省药品医疗器械检验研究院·河北省中药质量评价与标准研究重点实验室,河北 石家庄 050227;河北医科大学,河北 石家庄 050017
- 折叠
摘要
目的 建立参麦颗粒中红参掺伪的检查方法.方法 采用固相萃取-超高效液相色谱串联质谱(SPE-UPLC-MS/MS)法,色谱柱为Shimadzu Shim-pack GIST C18 柱(100 mm×2.1 mm,2 μm),流动相为乙腈-水(梯度洗脱),流速为 0.35 mL/min,柱温为40℃,进样量为5 μL.电喷雾离子源、负离子模式(ESI-),多反应监测(MRM)模式.结果 拟人参皂苷F11质量浓度在9.030～344.0 ng/mL范围内与峰面积线性关系良好(r = 0.999 2,n = 5),检测限和定量限分别为 1.128 8,22.8 ng/mL;精密度、稳定性、重复性试验结果的RSD均小于 4.0%;平均加样回收率为 108.17%,RSD为 4.24%(n = 6).以 0.051 μg/g为掺伪判定限度,3 家企业的 85 批样品中有9 批超出限度(检出率为 10.59%).结论 所建立的方法简便快速、准确度高、专属性强,可作为参麦颗粒中红参掺伪的检查方法.
Abstract
Objective To establish a method for adulteration detection of Ginseng Radix et Rhizoma Rubra in Shenmai Granules.Methods The solid-phase extraction ultra-high performance liquid chromatography tandem mass-spectrometry(SPE-UPLC-MS/MS)was adopted.The chromatographic column was Shimadzu Shim-pack GIST C18 column(100 mm×2.1 mm,2 μm),the mobile phase was acetonitrile-water(gradient elution),the flow rate was 0.35 mL/min,the column temperature was 40℃,and the injection volume was 5 μL.Multiple reaction monitoring(MRM)was adopted with electrospray negative ion source(ESI-).Results The linear range of pseudoginsenoside F11 was 9.030-344.0 ng/mL(r = 0.999 2,n = 5).The limit of detection and the limit of quantitation was 1.128 8,22.8 ng/mL respectively.The RSDs of precision,stability and repeatability tests were all lower than 4.0%.The average recovery rate of pseudoginsenoside F11 was 108.17%,with the RSD of 4.24%(n = 6).Taking 0.051 μg/g as the determination limit for adulteration,the concentration of pseudoginsenoside F11 in nine out of eighty-five batches of samples from three enterprises was over the limit,with the detection rate of 10.59%.Conclusion The established method is simple,fast,accurate and specific,which can be used for adulteration detection of Ginseng Radix et Rhizoma Rubra in Shenmai Granules.
关键词
参麦颗粒/红参/西洋参/掺伪/拟人参皂苷F11/固相萃取-超高效液相色谱串联质谱法Key words
Shenmai Granules/Ginseng Radix et Rhizoma Rubra/Panacis Quinquefolii Radix/adulteration/pseudoginsenoside F11/solid-phase extraction ultra-high performance liquid chromatography tandem mass-spectrometry引用本文复制引用
基金项目
中国药品监管科学行动计划重点项目(第二批)(NMPAJGKX-2023-024)
河北省重点研发计划(21372502D)
出版年
2024
国家科技期刊平台
NSTL
维普
万方数据