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1.上海中医药大学 中药研究所,中药标准化教育部重点实验室,上海 201203
2.上海中医药大学 中药学院, 上海 201203
3.北京清谱科技有限公司,北京 100084
李林楠,博士,副研究员,研究方向:中药复杂体系分离分析新技术、新方法及应用研究,E-mail:linnanli@shutcm.edu.cn
杨 莉,博士,研究员,研究方向:中药药效物质基础及质量标准,E-mail:yl7@shutcm.edu.cn
纸质出版日期:2025-02-15,
收稿日期:2024-07-30,
修回日期:2024-09-02,
录用日期:2024-10-22
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张丹,郑秀琴,斯子豪,王南,杨喜月,谷丽华,王峥涛,李林楠,杨莉.原位电离-便携质谱法对中药车前子掺伪葶苈子的现场快速筛查[J].分析测试学报,2025,44(02):221-228.
ZHANG Dan,ZHENG Xiu-qin,SI Zi-hao,WANG Nan,YANG Xi-yue,GU Li-hua,WANG Zheng-tao,LI Lin-nan,YANG Li.Ambient Ionization-Portable Mass Spectrometry for Rapid On-site Screening of Adulterated Descurainiae Semen in the Traditional Chinese Medicine Plantaginis Semen[J].Journal of Instrumental Analysis,2025,44(02):221-228.
张丹,郑秀琴,斯子豪,王南,杨喜月,谷丽华,王峥涛,李林楠,杨莉.原位电离-便携质谱法对中药车前子掺伪葶苈子的现场快速筛查[J].分析测试学报,2025,44(02):221-228. DOI: 10.12452/j.fxcsxb.240730264.
ZHANG Dan,ZHENG Xiu-qin,SI Zi-hao,WANG Nan,YANG Xi-yue,GU Li-hua,WANG Zheng-tao,LI Lin-nan,YANG Li.Ambient Ionization-Portable Mass Spectrometry for Rapid On-site Screening of Adulterated Descurainiae Semen in the Traditional Chinese Medicine Plantaginis Semen[J].Journal of Instrumental Analysis,2025,44(02):221-228. DOI: 10.12452/j.fxcsxb.240730264.
中药掺伪不仅严重影响药材质量,还可能导致临床疗效不佳,甚至引发不良反应或中毒事故。因此,防止或识别中药掺伪对确保药材质量和临床药效具有重要意义。该文采用纸毛细管喷雾电离结合便携质谱技术建立了车前子掺伪葶苈子的现场快速筛查方法。将样品粉末和萃取喷雾溶剂加入原位电离试剂盒中,萃取喷雾溶剂携带样品中的分析物在纸基质上向前移动,然后到达纸基质尖端发生离子化,最后进入便携质谱而被分析。分别考察了萃取喷雾溶剂、二级质谱碰撞能量、进样量、电喷雾电压对葶苈子中芥子碱硫氰酸盐响应强度的影响,最终选择甲醇作为萃取喷雾溶剂、二级质谱碰撞能量为1.3 V、进样量为23、电喷雾电压为4 500 V进行掺伪鉴别实验。同时,运用薄层色谱技术进一步验证便携质谱鉴别的准确性。实验结果表明,车前子与葶苈子的掺伪比例为1∶1至100∶1时,葶苈子中的特征成分芥子碱硫氰酸盐均可被检出。该方法无需繁琐的样品前处理过程,可在1 min内完成掺伪样品的现场即时筛查,可为车前子的市场规范及安全用药提供技术支持。
Adulteration of Chinese medicines not only seriously affects the quality of medicinal materials,but may also lead to poor clinical efficacy and even cause adverse reactions or poisoning. Therefore,it is of great significance to prevent or identify the adulteration of Chinese medicines to ensure the quality and clinical efficacy of medicinal materials. In this paper,we present a method for quickly screening for adulteration of Descurainiae Semen(DS) in Plantaginis Semen(PS) on-site,which utilizes paper capillary spray ionization(PCS) in conjunction with portable mass spectrometer (PMS). Sample powder and extraction spray solvent are added to PCS cartridge. The extraction spray solvent carries the target of sample forward on the paper matrix and thus reaches the tip of the paper matrix where ionisation occurs,and finally enters the cell portable mass spectrometer system for detection. We investigated the effects of extraction spray solvent,secondary mass spectrometry collision energy,injection volume,and electrospray voltage on the response intensity of Sinapine thiocyanate in DS,and finally chose methanol as the extraction spray solvent,an MS collision energy of 1.3 V,an injection size of 23,and an electrospray voltage of 4 500 V for the adulteration identification experiments. In addition,the accuracy of portable mass spectrometry identification was further validated using thin layer chromatography(TLC). The experimental results showed that sinapine thiocyanate in DS was detected when the adulteration ratio of PS to DS was from 1∶1 to 100∶1. The method does not require cumbersome sample handling and can complete the rapid screening of adulterated samples on the spot within 1 minute. This can support the standardization of PS in the market and ensure the safe use of medication by providing scientific evidence.
便携质谱纸毛细管喷雾电离快速鉴别中药掺伪车前子葶苈子
portable mass spectrometrypaper capillary spray ionizationrapid identificationadulteration of traditional Chinese medicinePlantaginis SemenDescurainiae Semen
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