Nat Prod Sci.  2016 Jun;22(2):93-101. 10.20307/nps.2016.22.2.93.

Qualitative and Quantitative Analysis of Thirteen Marker Components in Traditional Korean Formula, Samryeongbaekchul-san using an Ultra-Performance Liquid Chromatography Equipped with Electrospray Ionization Tandem Mass Spectrometry

• Seo CS
• Shin HK

• KMID: 2328873
• DOI: http://doi.org/10.20307/nps.2016.22.2.93

Abstract

For efficient quality control of the Samryeongbaekchul-san decoction, a powerful and accurate an ultra-performance liquid chromatography (UPLC) coupled with electrospray ionization (ESI) tandem mass spectrometry (MS) method was developed for quantitative analysis of the thirteen constituents: allantoin (1), spinosin (2), liquiritin (3), ginsenoside Rg1 (4), liquiritigenin (5), platycodin D2 (6), platycodin D (7), ginsenoside Rb1 (8), glycyrrhizin (9), 6-gingerol (10), atractylenolide III (11), atractylenolide II (12), and atractylenolide I (13). Separation of the compounds 1 - 13 was performed on a UPLC BEH C₁₈ column (2.1 × 100 mm, 1.7 µm) at a column temperature of 40 ℃ with a gradient solvent system of 0.1% (v/v) formic acid aqueous-acetonitrile. The flow rate and injection volume were 0.3 mL/min and 2.0 µL. Calibration curves of all compounds were showed good linearity with values of the correlation coefficient ≥ 0.9920 within the test ranges. The values of limits of detection and quantification for all analytes were 0.04 - 4.53 ng/mL and 0.13 - 13.60 ng/mL. The result of an experiment, compounds 2, 6, 12, and 13 were not detected while compounds 1, 3 - 5, and 7 - 11 were detected with 1,570.42, 5,239.85, 299.35, 318.88, 562.27, 340.87, 12,253.69, 73.80, and 115.01 µg/g, respectively.

Keyword

Qualitative analysis; Quantitative analysis; Samryeongbaekchul-san; UPLC; LC-MS/MS

MeSH Terms

Allantoin
Calibration
Chromatography, Liquid*
Glycyrrhizic Acid
Limit of Detection
Methods
Quality Control
Tandem Mass Spectrometry*
Allantoin
Glycyrrhizic Acid

Figure

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  Fig. 1. Chemical structures of the compounds 1–13 in Samryeongbaekchul-san.

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  Fig. 2. M ass spectra of the precursor ion (Q1, A) and product ion (Q3, B) for LC-MS/MS MRM mode of the compounds 1–13. Allantoin (1), spinosin (2), liquiritin (3), ginsenoside Rg1 (4), liquiritigenin (5), platycodin D2 (6), platycodin D (7), ginsenoside Rb1 (8), glycyrrhizin (9), 6-gingerol (10), atractylenolide III (11), atractylenolide II (12), and atractylenolide I (13).

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  Fig. 2. contineud

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  Fig. 2. contineud

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  Fig. 3. Total ion chromatograms of the standard solution (A) and Samryeongbaekchul-san sample (B) by LC-MS/MS MRM mode. Allantoin (1), spinosin (2), liquiritin (3), ginsenoside Rg1 (4), liquiritigenin (5), platycodin D2 (6), platycodin D (7), ginsenoside Rb1 (8), glycyrrhizin (9), 6-gingerol (10), atractylenolide III (11), atractylenolide II (12), and atractylenolide I (13).

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