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参麦颗粒中红参掺伪研究

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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。
Study on the Adulteration of Ginseng Radix et Rhizoma Rubra in Shenmai Granules
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.

Shenmai GranulesGinseng Radix et Rhizoma RubraPanacis Quinquefolii Radixadulterationpseudoginsenoside F11solid-phase extraction ultra-high performance liquid chromatography tandem mass-spectrometry

雷蓉、刘亚茹、王晓蕾、刘永利

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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

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

中国药品监管科学行动计划重点项目(第二批)河北省重点研发计划

NMPAJGKX-2023-02421372502D

2024

中国药业
重庆市食品药品监督管理局

中国药业

CSTPCD
影响因子:1.369
ISSN:1006-4931
年,卷(期):2024.33(8)
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