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HPLC-CAD
ANALYTICAL AND BIOANALYTICAL CHEMISTRY · 2023 ·Vol. 415 ·期 17 ·3375-3384 · IF 4.3

HPLC-CAD as a supplementary method for the quantification of related structure impurities for the purity assessment of organic CRMs

Liu Si,Lu Boling,Peng Zijuan,Liu Chunyu,Liu Yuhui,Jiao Hui,Wu Dan,Li Penghui,Zhao Xingchen,Song Shanjun

In organic purity assessment, chromatography separation with a suitable detector is required. Diode array detection (DAD) has been a widely used technique for high-performance liquid chromatography (HPLC) analyses, but its application is limited to compounds with sufficient UV chromophores. Charged aerosol detector (CAD), as a mass-dependent detector, is advantageous for providing a nearly uniform response for analytes, regardless of their structures. In this study, 11 non-volatile compounds with/without UV chromophores were analyzed by CAD using continuous direct injection mode. The RSDs of CAD responses were within 17%. For saccharides and bisphenols, especially, the RSDs were lower ( 2.12% and 8.14%, respectively). Since bisphenols exist in UV chromophores, their HPLC–DAD responses were studied and compared with CAD responses, with CAD showing a more uniform response. Besides, the key parameters of HPLC-CAD were optimized and the developed method was verified using a Certified Reference Material (CRM, dulcitol, GBW06144). The area normalization result of dulcitol measured by HPLC-CAD was 99.89% ± 0.02% ( n  = 6), consistent with the certified value of 99.8% ± 0.2% ( k  = 2). The result of this work indicated that the HPLC-CAD method could be a good complementary tool to traditional techniques for the purity assessment of organic compounds, especially for compounds lacking UV chromophores. Graphical Abstract

研究领域: 分析化学 · 药物分析
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Journal of Oleo Science · 2025 · IF 1.8

Quantification of Fatty Acids from Arctium lappa L. Leaves by 13C qNMR and HPLC-CAD

Weijie Shang,Yanjie Huang,Yihang Zhang,Ruojia Li,Liping Dai

Arctium lappa L. (burdock) leaves is effective in the traditional treatment of stroke. Fatty acids are abundant in burdock leaves, and may play an important role in the treatment of stroke. A new procedure was presented that provides 13C NMR-based quantitative measurements of total content, average chain length, average degree of unsaturation, and average polyunsaturation of fatty acids in burdock leaves from five producing areas. The content of five fatty acids in burdock leaves, including α-linolenic acid, linoleic acid, palmitic acid, oleic acid, and stearic acid, were further determined by HPLC-CAD. Among five producing areas, the results of 13C qNMR showed that the content of total fatty acids in burdock leaves ranged from 8.62 to 24.51 μmol·g–1, the average chain length ranged from 19.67 to 23.14, the average degree of unsaturation ranged from 1.19 to 3.91, and the average polyunsaturated moieties ranged from 0.23 to 2.37. The results of HPLC-CAD showed that the contents of α-linolenic acid, linoleic acid, palmitic acid, oleic acid and stearic acid were 0.66 - 6.60 mg·g–1, 0.38-4.41 mg·g–1, 0.46-3.55 mg·g–1, 0.18-0.20 mg·g–1 and 0.10-0.32 mg·g–1 respectively. The developed 13C qNMR method can accurately determine the total fatty acids content and provide relevant information on the fatty acids structure types in burdock leaves. This method is capable of complementing existing fatty acids quantitative methodologies, circumventing their deficiencies, and its application can be extended to other plants.

CAS / MDL: 100-25-4
研究领域: 天然产物化学 · 代谢组学 · 植物化学 · 分析化学 · 药用植物学
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MICROCHIMICA ACTA · 2025 ·Vol. 192 ·期 10 ·1-12 · IF 5.3

Development of three-dimensional boronate affinity dendritic mesoporous silica coupled with HPLC-CAD for selective determination of ginsenosides

Zhao Weiman,Fan Wenxiang,Liu Longchan,Gao Yingrui,Tong Ruonan,You Liying,Li Linnan,Wang Zhengtao,Yang Li

The precise and selective determination of ginsenosides, pharmacologically diverse saponins abundant in Panax species, is crucial for their therapeutic development and stringent quality control. However, inherent challenges, including their weak ultraviolet absorption and the high polarity imparted by sugar moieties, complicate their determination. Addressing these limitations, this study introduces the first-time construction and application of a boronate affinity dendritic mesoporous silica nanomaterial (BA-DMSN) as a highly efficient adsorbent for ginsenoside pretreatment. The synthesized BA-DMSN was comprehensively characterized, confirming a unique three-dimensional open dendritic framework, high specific surface area, and exceptional inner surface accessibility. These attributes facilitate rapid analyte adsorption and release, enabling a solid-phase extraction (SPE) process completed within approximately 10 min. Critically, the strategic incorporation of boronic acid groups conferred specific selectivity towards the cis-diol structures present in ginsenosides, allowing for their highly effective enrichment from complex matrices. Integrating this novel adsorbent with charged aerosol detection (CAD), a boronate affinity chromatography strategy was successfully developed and validated for the quantitative determination of nine key ginsenosides (notoginsenosides Fa, Fc, FP2, Fe, and ginsenosides Rc, Rd, Rb1, Rb2, Rb3) in stem-leaf extracts of Panax notoginseng. Methodological investigations demonstrated that this approach offers significant advantages over existing techniques, including operational simplicity, outstanding selectivity, and enhanced sensitivity, particularly for ginsenosides lacking strong chromophores. The successful analysis of actual Panax notoginseng samples underscores the robust applicability and promising prospects of the BA-DMSN-based SPE-CAD methodology for the quality control and further research of ginsenoside-based natural products. Graphical

CAS / MDL: 958-09-8
研究领域: 分析化学 · 纳米材料 · 植物化学 · 药物分析 · 天然产物研究
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Natural Product Communications · 2024 · IF 1.5

Isolation and Identification of Anti-Inflammatory Active Components from Asparagi Radix cochinchinensis Based on HPLC-CAD and UPLC-Q/TOF-MS Techniques

Yan Lei,Bing Wang,Guanglin Zhu,Guo Feng,Wei Li,Caiyao Han,Qian Qin,Xie-an Yu,Xueli Song,Zhengyan He,Ju Zhang,Hongmei Su,Wenjing Wang

Background: In the research of the pharmacological activity of modern Chinese medicine, a large number of traditional Chinese medicines show anti-inflammatory activity. Asparagi radix is one of the anti-inflammatory drugs. With the deepening of people's research on Asparagi radix, its anti-inflammatory pharmacological effects have been gradually explored, but its specific anti-inflammatory active ingredients are still unclear. Therefore, it is necessary to screen and identify its specific anti-inflammatory active ingredients from Asparagi radix. At present, COX-2 is an important target for the treatment of chronic inflammation, and many drugs targeting this target have been marketed. However, some drugs have serious side effects, so it is very meaningful to study new COX-2 inhibitors. Methods: In this experiment, the fractions of different time periods are separated by high performance liquid chromatography-separation-trapping system (HPLC-CAD-FC). Then, ultra-high performance liquid chromatography-quadrupole time-of-flight/mass spectrometry (UPLC-Q-TOF/MS) and biological activity analysis techniques are used to identify the chemical composition and in vitro anti-inflammatory activity of each fraction. Finally, the data is integrated to screen out the substances with potential anti-inflammatory activity in Asparagi radix. Results: The results showed that the method established in this experiment can successfully isolate the active components of Asparagi radix, and four saponins with potential anti-inflammatory activity are identified. Conclusion: In summary, the analysis method established in this study can quickly and effectively screen out its anti-inflammatory active substances, and its potential anti-inflammatory active ingredients are mainly steroidal saponins.

CAS / MDL: 64-18-6
研究领域: 中药学 · 药理学
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