Forsythia suspensa Fruit

Forsythia Species Fruit

Proposed For Development Version 0.1

Forsythia suspensa Fruit

 


 

DEFINITION

The article consists of the dried fruit of Forsythia suspensa (Thunb.) Vahl. (Family Oleaceae). It contains NLT 2.4% of total lignans and phenylethanoids calculated as the sum of forsythiaside, lariciresinol, phillyrin, pinoresinol, and phillygenin on the dried basis.

 

SYNONYMS

Forsythia fortunei Lindl.

Forsythia giraldiana f. pubesces (Rehder) C.C.Niu

Forsythia sieboldii (Zabel) Dippel

Forsythia suspensa f. atrocaulis Rehder

Forsythia suspensa f. aureovariegata Koehne

Forsythia suspensa f. decipiens Koehne

Forsythia suspensa var. fortunei (Lindl.) Rehder

Forsythia suspensa f. pallida Koehne

Forsythia suspensa f. pubescens Rehder

Forsythia suspensa var. pubescens (Rehder) Lingelsh.

Forsythia suspensa var. sieboldii Zabel

Forsythia suspensa f. variegata Butz. Ex Rehder

Ligustrum suspensum Thunb.

Lilac perpensa Lam.

Rangium suspensum (Thunb.) Ohwi

Syringa suspensa Thunb.

 

POTENTIAL CONFOUNDING MATERIALS

Forsythia viridissima Linl.

 

SELECTED COMMON NAMES

Chinese: 连翘

English: Forsythia, golden-bell, goldenbells, weeping forsythia, weeping goldenbells

Korean: 연교

Swedish: Hängforsythia

 

CONSTITUENTS OF INTEREST

Lignans: Forsythiaside, phillyrin, phillygenin, pinoresinol, lariciresinol

 

IDENTIFICATION

• A. Botanical Characteristics: To Come

 

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

Standard solution: 0.6 mg/mL each of USP Forsythiaside RS, USP Lariciresinol RS, USP Phillyrin RS, USP Pinoresinol RS, and USP Phillygenin RS in methanol

Sample solution: 100 mg of Forsythia suspensa Fruit, finely powdered, in 50 mL of 70% methanol. Sonicate for 10 min, and use the supernatant or filtrate.

Chromatographic system

Adsorbent: Use a suitable chromatographic material with an average particle size of 5 µm (HPTLC plates).

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: Methanol and water (60:40)

Developing distance: 6 cm

Derivatization reagent: 10% sulfuric acid

System suitability: To Come

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 saturated chamber (20 min with filter paper), remove the plate from the chamber, and examine under UV light at 254 and 366 nm. Then treat the plate with 10% sulfuric acid and heat at 100° for 2 min.

Acceptance criteria: After derivatization, the Sample solution of Forsythia suspensa Fruit exhibits the most intense quenching band in the upper section, corresponding in RF to the forsythiaside, lariciresinol, phillyrin, pinoresinol, and phillygenin band in the Standard solution.

 

· C. HPLC

Analysis: Proceed as directed in the Assay for Content of Total Lignans and Phenylethanoids.

Samples: Standard solutions A–E and Sample solution

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

 

ASSAY

• Content of Total Lignans and Phenylethanoids

Solution A: 3% acetic acid in water

Solution B: Methanol

Mobile phase: See Table 1.

 

Table 1

Time
(min)

Solution A
(%)

Solution B
(%)

0

70

30

8

67

33

24

60

40

39

57

43

55

30

70

60

5

95

70

5

95

85

70

30

100

70

30

 

Solvent: Methanol and water (50:50)

Standard solution A: 0.036 mg/mL of USP Forsythiaside RS in methanol

Standard solution B: 0.002 mg/mL of USP Lariciresinol RS in methanol

Standard solution C: 0.004 mg/mL of USP Phillyrin RS in methanol

Standard solution D: 0.002 mg/mL of USP Pinoresinol RS in methanol

Standard solution E: 0.002 mg/mL of USP Phillygenin RS in methanol

Sample solution: Accurately transfer about 100 mg of finely powdered Forsythia suspensa Fruit to a 100-mL centrifugal tube, add 50 mL of Solvent, and weigh. Sonicate for 60 min, cool, and compensate the weight loss with Solvent. Before injection, pass through a membrane filter of 0.45-μm popre size.

Chromatographic system

(See Chromatography <621>, System Suitability.)

Detector: UV 280 nm

Column: 4.6-mm × 25-cm; 5-μm packing L1

Flow rate: 1.0 mL/min

Injection volume: 10 µL

System suitability: To Come

Analysis

Samples: Standard solutions A–E and Sample solution

Calculate the percentage of forsythiaside, lariciresinol, phillyrin, pinoresinol, and phillygenin in the portion of Forsythia suspensa Fruit taken:

 

Result = (rU/rS) × CS × (V/W) × 100

 

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

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

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

V    = volume of the Sample solution, mL

W   = weight of Forsythia suspensa Fruit taken to prepare the Sample solution, mg

 

Acceptance criteria: NLT 2.4% of the sum of forsythiaside, lariciresinol, phillyrin, pinoresinol, and phillygenin for Forsythia suspensa Fruit on the dried basis

 

CONTAMINANTS

• Elemental Impurities—Procedures <233>

Acceptance criteria

Arsenic: NMT 3 µg/g

Cadmium: NMT 0.3 µg/g

Lead: NMT 5 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

 

SPECIFIC TESTS

• Articles of Botanical Origin  <561>, Methods of Analysis, Foreign Organic Matter: NMT 2.0%

• 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 5.0%

• 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 Forsythiaside RS

USP Lariciresinol RS

USP Phillygenin RS

USP Phillyrin RS

USP Pinoresinol RS

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