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. 2024 Apr 30;15:1366556. doi: 10.3389/fphar.2024.1366556

TABLE 1.

Application of modern analytical techniques in quantitative analysis of quality control of Codonopsis Radix.

No. Species Chemical component Part Extraction methods Analysis Technique References
1 C. pilosula Lobetyolin, Syringin, Atractylenolide III leaves, roots 1 g powder was extracted with 50/25 mL of 75%/100% methanol, ultrasonication (power: 100  W, frequency: 40 KHz) for 30/45 min (Lobetyolin/ Syringin,Atractylenolide III). LC- MS/MS: Agilent C18 (2.1 mm × 100 mm, 3 μm) column at 35°C, and the flow rate was 0.3 mL/min. Mobile phase consisting of (A) 0.1% formic acid and (B) methanol. In negative ESI mode, on spray voltage, 5500 V; collision energy, 30 V; and capillary temperature, 550°C. (Lobetyolin). Zeng et al. (2022)
HPLC: Agela venusil ASB-C18 (4.6 mm × 250 mm, 5 μm) at room temperature and the flow rate was 0.8 mL/min. Mobile phase consisting of (A) 0.1% phosphoric acid solution and (B) acetonitrile. The detection wavelength was 220 nm. (Syringin, Atractylenolide III)
2 C. pilosula, C. pilosula var. Modesta, C. tangshen D-fructose, Glucose, Sucrose, FOS (GF2–GF6) roots 0.1 g powder was extracted with 20 mL of 60 % methanol, ultrasonication (power: 250 W, frequency: 40 KHz) for 60 min. HPLC-CAD: Waters XBridge™ Amide column (4.6 × 250 mm, 3.5 μm, Waters Corp.) and the flow rate was 1.0 mL/min. Mobile phase consisting of (A) acetonitrile and (B) 0.1% triethylamine aqueous solution. CAD detector: nitrogen gas pressure, 55.0 pa; data collection rate, 10 Hz; and noise filter, 5.0 s. Xie et al. (2022)
3 C. pilosula, C. pilosula var. Modesta, C. tangshen Lobetyolin, total flavonoids, pigments, total solid contents roots 89-95% ethanol extraction FT-NIR: Instrument resolution is specified at 4 cm−1. Each spectrum was acquired by averaging 64 scans across the wavenumber range of 4000–10000 cm-1, while background spectra were obtained against air. The samples were equilibrated to room temperature (25°C) prior to NIR spectra collecting. Luo et al. (2017)
HPLC: Agela venusil ASB-C18 (4.6 mm × 250 mm, 5 μm) at 30°C and the flow rate was 1.0 mL/min. Mobile phase consisting of 20% acetonitrile-water (v/v). The detection wavelength was set at 269 nm. (lobetyolin).
Sodium nitrite-aluminium nitrate and tartrazine colorimetric methods were used to quantify total flavonoids and pigments, respectively.
4 C. pilosula, C. pilosula var. Modesta, C. tangshen Lobetyolin roots 1.0 g powder was extracted with 25 mL of 60 % methanol, ultrasonication (power: 200 W, frequency: 40 KHz) for 30 min. HPLC: Elite C18 (4.6 mm × 250 mm, 5 μm) at 25°C and the flow rate was 0.8 mL/min. Mobile phase consisting of (A) 0.1% phosphoric acid solution and (B) acetonitrile. The detection wavelength was 220 nm. Gu et al. (2016)
5 C. pilosula, C. pilosula var. Modesta, C. tangshen Lobetyol, Lobetyolin, tangshenoside I roots 50 mg powder was extracted with 30 mL of 70 % methanol, ultrasonication for 60 min. HPLC-DAD: YMC-Pack Pro-C18-column (4.6 mm i.d. × 250 mm, 5 µm) at room temperature. and the flow rate was 1.0 mL/min. Mobile phase consisting of (A) a water-1.0 % aqueous solution of 0.1 M phosphoric acid and (B) an acetonitrile-1.0 % aqueous solution of 0.1 M phosphoric acid. The detection wavelength was 267 nm. Kim et al. (2014)
6 C. pilosula, C. pilosula var. Modesta, C. tangshen Codonopyrrolidium B, Codonopyrrolidium A, Tangshenoside I, Cordifolioidyne B, Lobetyolinin, Lobetyolin, Lobetyol roots 1.0 g powder was extracted with 15 mL of methanol, ultrasonication for 20 min. HPLC-DAD: Kromasil C18 column (4.6 mm × 250 mm, 5 μm) at 30 °C and the flow rate was 1.0 mL/min. Mobile phase consisting of (A) acetonitrile and (B) 0.1% phosphoric acid. The detection wavelength was 215 nm. He et al. (2014a)
7 C. pilosula, C. pilosula var. Modesta, C. tangshen Codonopyrrolidium B, codonopyrrolidium A, tangshenoside I, cordifolioidyne B, lobetyolinin, lobetyolin, lobetyol roots 1.0 g powder was extracted with 15 mL of methanol, ultrasonication for 20 min. HPLC-DAD:Kromasil C18 column (4.6 mm × 250 mm, 5 μm) at 30 °C and the flow rate was 1.0 mL/min. Mobile phase consisting of (A) acetonitrile and (B) 0.1% phosphoric acid. The detection wavelength was 215 nm. He et al. (2014b)
8 C. pilosula, C. pilosula var. Modesta, C. tangshen Codonopyrrolidum B, Histidine, 4-hydroxy benzoic acid, tangshenoside I, codonopyrrolidum A, lobetyolin, codonoside A, tetradeca-4E,8E,12E-triene-10-yne-1,6,7-triol, lobetyol roots sat. n-BuOH (n-BuOH pre-saturated with H2O)/H2O, collected partition layer was dried. HPLC: Dianion HP-20 column and semi-preparative HPLC separation, at 30 °C. Mobile phase consisting of (A) acetonitrile and (B) 0.1% formic acid. The detection wavelength was 254 nm. Lin et al. (2013)
9 C. pilosula, C. pilosula var. Modesta, C. tangshen Lobetyolin roots 1.0 g powder was extracted with 50 mL of methanol, ultrasonication for 60 min. HPLC: C18 column (4.6 mm × 250 mm, 5 μm) at 25 °C and the flow rate was 1.0 mL/min. Mobile phase consisting of (A) acetonitrile and (B) water. The detection wavelength was 270 nm. Qing-Wen et al. (2009)
10 C. pilosula, C. pilosula var. Modesta, C. tangshen Codonopsine, Codonopsinine, codotubulosine A, codotubulosine B, adenosine, 5-(hydroxymethyl)furfural roots 1.0 g powder was extracted with 10 mL of water, ultrasonication for 30 min at room temperature. (Three times) NMR: 1H NMR spectra were recorded in methanol-d4 (99.9%) using a Varian UNITY plus 400 MHz spectrometer. For each sample, 200 scans were recorded with the following parameters: 0.187 Hz/point; spectra width, 14,400 Hz; pulse width, 4.0 μs; relaxation delay, 1 s. Li et al. (2009)
11 C. pilosula, Tangshenoside I, lobetyolin, lobetyol roots 1.0 g powder was extracted with 25 mL of methanol, was then extracted by refluxing for 120 min. HPLC: A Zorbax XDB RP-C18 column at 20 °C. Mobile phase consisting of (A) acetonitrile and (B) water. The detection wavelength was 267 and 295 nm. Qiao et al. (2007)
12 C. pilosula, C. pilosula var. Modesta, C. tangshen Atractylenolide III roots 2.0 g powder was extracted with 50 mL of methanol, ultrasonication for 30 min. HPLC: Kromasil C18 column (4.6 mm × 250 mm, 5 μm) and the flow rate was 0.80 mL/min. Mobile phase consisting of (A) methanol and (B) water. The detection wavelength was 220 nm. Hao et al. (2002)
13 C. pilosula Atractylenolide III roots 5.0 g powder was extracted with 25 mL of methanol, ultrasonication for 30 min. N-Butanol extraction. HPLC-ELSDA, HPLC-PDA: HypersilODS-2 C18 column (4.6 mm × 250 mm, 5 μm) and the flow rate was 1.0 mL/min. Mobile phase consisting of (A) methanol and (B) water. The detection wavelength was 220 nm. Li et al. (2005)
14 C. pilosula, C. pilosula var. Modesta, C. tangshen Atractylenolide III, lobetyolin roots 0.6 g powder was extracted with 10 mL of n-hexane/ethanol, ultrasonication. The extract was evaporated to dryness and dissolved in methanol. (Atractylenolide III/ lobetyolin) HPLC-PDA: C18 column (4.6 mm × 250 mm, 5 μm) at 25 °C and the flow rate was 1.0 mL/min. Mobile phase consisting of (A) acetonitrile and (B) water/0.1% acetic acid. The detection wavelength was 220/267.3 nm. (Atractylenolide III/ lobetyolin) Pang et al. (2008)
15 C. pilosula, C. pilosula var. Modesta, C. tangshen Lobetyolin roots 4.0 g powder was extracted with 100 mL of methanol, soxhlet extraction for 30 min. The extract was evaporated to dryness and dissolved in methanol. HPLC-PDA: Supelco Discovery C18 column (4.6 mm × 250 mm, 5 μm) at 30 °C and the flow rate was 1.0 mL/min. Mobile phase consisting of (A) acetonitrile and (B) 0.5% acetic acid. The detection wavelength was 268 nm. Song et al. (2008)
16 C. pilosula Lobetyolin Stems, leaves, flowers 0.5 g powder was extracted with 10 mL of methanol, ultrasonication (power: 250 W, frequency: 20 KHz) for 40 min. HPLC: Merck Purospher Star LP RP-8 endcapped (4.6 mm × 250 mm, 5 μm) at 30 °C and the flow rate was 1.0 mL/min. Mobile phase consisting of (A) acetonitrile and (B) water. The detection wavelength was 490 nm. Cheng et al. (2020b)
17 C. pilosula Lobetyolin roots 1.0 g powder was extracted with 50 mL of methanol, ultrasonication (power: 100 W, frequency: 40 KHz) for 40 min. HPLC-DAD: Sunfire C18 column (4.6 mm × 250 mm, 5 μm) at 30 °C and the flow rate was 1.0 mL/min. Mobile phase consisting of (A) methanol and (B) water. The detection wavelength was 267 nm. Duan et al. (2012)
18 C. pilosula, C. pilosula var. Modesta, C. tangshen Syringin, tangshenoside I, lobetyolin, atractylenolide III roots 1.0 g powder was extracted with 25 mL of methanol, ultrasonication (power: 250 W, frequency: 59 KHz) for 30 min. The extract was evaporated to dryness and dissolved in methanol. HPLC: InertSustainl C18 column (4.6 mm × 250 mm, 5 μm) at 30°C and the flow rate was 0.8 mL/min. Mobile phase consisting of (A) acetonitrile and (B) 0.2% phosphoric acid. The detection wavelength was 220 nm. Zhang et al. (2022)
19 C. pilosula, C. pilosula var. Modesta, C. tangshen Adenosine, Tryptophan, Syringin, tangshenoside I, Lobetyolin, Atractylenolide III roots 2.0 g powder was extracted with 20 mL of 70% methanol, ultrasonication (power: 140 W, frequency: 42 KHz) for 30 min. HPLC: ACE Neptune-C18 column (4.6 mm × 250 mm, 5 μm) at 20 °C and the flow rate was 0.8 mL/min. Mobile phase consisting of (A) acetonitrile and (B) 0.15 % formic acid. The detection wavelength was 260 nm. Huang et al. (2022)
20 C. pilosula, C. pilosula var. Modesta, C. tangshen Lobetyolin, syringin roots 1.0 g powder was extracted with 50 mL of methanol, immersing 15 min and ultrasonication for 30 min. The extract was evaporated to dryness and dissolved in methanol. HPLC: Thermo scientific C18 column (4.6 mm × 250 mm, 5 μm) at 25 °C and the flow rate was 1.0 mL/min. Mobile phase consisting of (A) acetonitrile and (B) water. The detection wavelength was 266 nm. Chen et al. (2016)
21 C. tangshen Lobetyolin, Atractylenolide III, Protocatechuic acid, Succinic acid, Adenosine Phenylalanine, Tyrosine, Tryptophan roots 1.0 g powder was extracted with 25 mL of 50% methanol, ultrasonication for 60 min. UPLC-MS: Acquity UPLC BEH-C18 column (2.1 mm × 100 mm, 1.7 μm) at 35 °C and the flow rate was 0.3 mL/min. Mobile phase consisting of (A) acetonitrile and (B) 0.1 % formic acid. In positive/negative ESI mode, on spray voltage, 2000 V; collision energy, 40 eV; and capillary temperature, 320°C. An et al. (2018)
22 C. pilosula, C. pilosula var. Modesta, C. tangshen Lobetyolin, Tangshenoside Ⅳ, Atractylenolide III. roots 5.0 g powder was extracted with 50 mL of methanol, ultrasonication for 30 min. The extract was evaporated to dryness and dissolved in methanol. The extract was evaporated to dryness and dissolved in methanol. HPLC: Elite SinoChrom ODS-BP C18 column (4.6 mm × 250 mm, 5 μm) at 25°C and the flow rate was 1.0 mL/min. Mobile phase consisting of (A) acetonitrile and (B) water. The detection wavelength was 266 nm. Li et al. (2011)