Angelica gigas Root Powder

Angelica gigas Root Powder

Proposed For Development Version 0.1

Angelica gigas Root Powder

 


 

DEFINITION

 

The article consists of the dried roots of Angelica gigas Nakai (Family Apiaceae), reduced to powder or very fine powder. It contains NLT 4.2% of caffeoylquinic acid and total coumarins calculated as the sum of chlorogenic acid, demethylsuberosin, decursin, and decursinol angelate on the dried basis.

 

POTENTIAL CONFOUNDING MATERIALS

Angelica acutiloba (Siebold & Zucc.) Kitag.

Angelica sinensis (Oliv.) Diels

 

CONSTITUENTS OF INTEREST

Coumarins: Decursin, decursinol, decursinol angelate, nodakenin

 

IDENTIFICATION

• A. Botanical Characteristics: To Come

 

· B. HPTLC for Articles of Botanical Origin <203>

Standard solution: 1.0 mg/mL each of USP Imperatorin RS, USP Osthole RS, and USP Isoimperatorin RS in methanol

Sample solution: 1 g of Angelica gigas Root Powder in 5 mL of methanol. Sonicate for 10 min and centrifuge or filter. Use supernatant or filtrate.

Chromatographic system

Adsorbent: Chromatographic silica gel F254 mixture

Application volume: 10 µL each of Standard solution and Sample solution, as 8-mm bands

Relative Humidity: Condition the plate to a relative humidity of about 33% using a suitable device

Developing solvent system: Toluene, ethyl acetate, and acetic acid (90:10:1)

Developing distance: 6 cm

Analysis

Samples: Standard solution and Sample solution

Apply the Samples as bands to a suitable HPTLC plate and dry in air. Develop the chromatograms in a saturated chamber (20 min with filter paper), remove the plate from the chamber, and examine under UV 365 nm light.

System suitability: To Come

Acceptance criteria: Under UV 365 nm light, the chromatogram of the Sample solution exhibits about 8 fluorescence bands in the lower half of the chromatogram. Three pale fluorescence bands appear above the broad fluorescence band near RF 0.25 corresponding in color and RF to the bands due to imperatorin, osthole, and isoimperatorin, with increasing RF in the Standard solution

 

· C. HPLC

Analysis: Proceed as directed in the Assay for Content of Caffeoylquinic Acid and Total Coumarins. 

Acceptance criteria: The Sample solution exhibits the most intense peak at a retention time corresponding to each Standard solution.

 

ASSAY

• Content of Caffeoylquinic Acid and Total Coumarins

Solution A: 0.1% formic acid in water

Solution B: 0.1% formic acid in acetonitrile

Mobile phase: See Table 1.

 

Table 1

Time
(min)

Solution A
(%)

Solution B
(%)

0

88

12

10

82

18

25

80

20

30

50

50

60

50

50

 

Solvent: Ethyl alcohol and water (7:3)

Standard solution A: 0.2 mg/mL  of USP Chlorogenic Acid RS in methanol

Standard solution B: 0.8 mg/mL of USP Demethylsuberosin RS in methanol

Standard solution C: 2 mg/mL of USP Decursin RS in methanol

Standard solution D: 2 mg/mL of USP Decursinol Angelate RS in methanol

Sample solution: Accurately transfer about 1.0 g of Angelica gigas Root Powder to a centrifugal tube, add 10 mL of Solvent, and weigh. Sonicate for 45 min, cool, and compensate the weight loss with Solvent. Before injection, pass through a membrane filter of 0.45-μm pore size.

Chromatographic system

(See Chromatography <621>, System Suitability.)

Detector: UV 325 nm

Column: 4.6-mm × 25-cm; packing L1

Column temperature: 40°

Flow rate: 1.0 mL/min

Injection volume: 10 µL

System suitability: To Come

Analysis

Samples: Standard solutions A–D and Sample solution

Calculate the percentage of chlorogenic acid, demethylsuberosin, decursin, and decursinol angelate in the portion of Angelica gigas Root Powder taken:

 

Result = (rU/rS) × CS × (V/W) × 100

 

rU   = peak area of the corresponding analyte from the Sample solution

rS   = peak area of the corresponding analyte from the Standard solution

CS  = concentration of the Standard solution (mg/mL)

   = volume of the Sample solution, mL

W   = weight of Angelica gigas Root Powder taken to prepare the Sample solution, mg

 

Acceptance criteria: NLT 4.2% of caffeoylquinic acid and coumarins on the dried basis

 

CONTAMINANTS

• Elemental Impurities—Procedures <233>

Acceptance criteria

Arsenic: NMT 3.0 µg/g

Cadmium: NMT 0.3 µg/g

Lead: NMT 5.0 µg/g

Mercury: NMT 0.2 µg/g

• Articles of Botanical Origin <561>, Pesticide Residue Analysis: Meets the requirements

• Microbial Enumeration Tests <61>: The total aerobic bacterial count does not exceed 105 cfu/g, the total combined molds and yeasts count does not exceed 103 cfu/g, and the bile-tolerant Gram-negative bacteria does not exceed 103 cfu/g.

• Tests for Specified Microorganisms <62>: Meets the requirements of the tests for absence of Salmonella species and Escherichia coli

• Articles of Botanical Origin <561>, Test for Aflatoxins: Meets the requirements

 

SPECIFIC TESTS

• Articles of Botanical Origin <561>, Methods of Analysis, Foreign Organic Matter: NMT 5.0%

• Articles of Botanical Origin <561>, Methods of Analysis, Alcohol-Soluble ExtractivesMethod 1: To Come

• Articles of Botanical Origin <561>, Methods of Analysis, Water-Soluble ExtractivesMethod 2: To Come

• Loss on Drying <731>: To Come

• Articles of Botanical Origin <561>, Methods of Analysis, Total Ash: NMT 6.0%

• Articles of Botanical Origin <561>, Methods of Analysis, Acid-Insoluble Ash: To Come

 

ADDITIONAL REQUIREMENTS

• Packaging and Storage: Preserve in well-closed containers, protected from light and moisture, and store at room temperature.

• Labeling: The label states the Latin binomial and the part(s) of the plant contained in the article.

• USP Reference Standards <11>

USP Chlorogenic Acid RS

USP Decursin RS

USP Decursinol Angelate RS

USP Demethylsuberosin RS

USP Imperatorin RS

USP Isoimperatorin RS

USP Osthole RS

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