Schisandra chinensis Fruit Powder

Schisandra chinensis Fruit Powder

Proposed For Development Version 0.1

Schisandra chinensis Fruit Powder

 


 

DEFINITION

 

The article consists of dried ripe fruits of Schisandra chinensis (Turcz.) Baill. (Family Schisandraceae) reduced to a fine or very fine powder. It contains NLT 0.95% of lignans, calculated as the sum of schisandrin (C24H32O7), schisandrol B (C23H28O7), deoxyschisandrin C24H32O6), and γ-schisandrin (C23H28O6) on the dried bases.

 

SYNONYMS

Kadsura chinensis Turcz.

Maximowiczia amurensis Rupr.

Maximowiczia chinensis (Turcz.) Rupr.

Maximowiczia japonica (A.Gray) K. Koch

Maximowiczia sinensis Rob.

Sphaerostema japonicum A.Gray

 

POTENTIAL CONFOUNDING MATERIALS

Kadsura japonica (L.) Dunal

Schisandra sphenanthera Rehder & E. H. Wilson

 

SELECTED COMMON NAMES

Chinese: 五味子, 北五味子

English: Schisandra, Northern schisandra, Chinese magnolia vine, five flavor fruit, magnolia vine

Finnish: Palsamiköynnös

French: Schisandra de Chine

German: Chinesisches Spaltkölbchen, Chinesischer Limonenbaum

Japanese: ゴミシ

Korean: 오미자

Pinyin: Wu Wei Zi, Bei Wu Wei Zi

Russian: Лимонник китайский

Swedish: fjärilsranka

 

CONSTITUENTS OF INTEREST

Lignans: Schisandrin, schisandrol B, deoxyschisandrin, γ-schisandrin

 

IDENTIFICATION

• A. Botanical Characteristics

Macroscopic: Dark purple in color

Microscopic: The epidermal stone cells of testa are polygonal or elongated-polygonal in surface view, 18-50 μm in diameter, thickened walls with very fine and densed pit canals; within the cells containg dark brown contents. The inner layer stone cells of testa are polygonal, subrounded or irregular, up to 83 μm in diameter, slightly thickened walls with relatively large pits. Epidermal cells of pericarp are polygonal in surface view, anticlinal walls slightly beaded with cuticle striations (unlike Schisandra sphenanthera, where anticlinal walls are not beaded), scattered with oil cells. Cells in mesocarp are shriveled, containing dark brown contents and starch granules.

  

B. Thin-Layer Chromatography

Standard solution A: 1.0 mg/mL of USP Schisandrin RS in ethanol

Standard solution B: Sonicate 500 mg of USP Schisandra chinensis Fruit Dry Extract RS in 10 mL of ethanol for 10 min. Centrifuge, evaporate the supernatant under reduced pressure to dryness. Dissolve the residue in 1 mL of ethanol with sonication, centrifuge, and use the supernatant.

Sample solution: Sonicate 1.0 g of Schisandra chinensis Fruit Powder in 10 mL of ethanol for 10 min. Centrifuge, evaporate the supernatant under reduced pressure to dryness. Dissolve the residue in 1 mL of ethanol with sonication, centrifuge, and use the supernatant.

Chromatographic system

(See Chromatography <621>, Thin-Layer Chromatography.)

Adsorbent: Chromatographic silica gel F254 mixture with an average particle size of 5 µm (HPTLC plates).

Application volume: 3 µL as 8-mm bands

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

Developing solvent system: A mixture of toluene, ethyl acetate, and glcial acetic acid (23:6:1)

Developing distance: 6 cm

Analysis

Samples: Standard solution A, Standard solution B, and Sample solution

Apply the samples as bands to a suitable high performance thin-layer chromatographic plate and dry in air. Develop the chromatograms in a saturated chamber, remove the plate from the chamber, dry, and examine under UV light  at 254 nm.

System suitability: Under UV light at 254 nm , the chromatogram of Standard solution B exhibits six bands in the lower-third section; the most intense band corresponds in RF to the band due to schisandrin in the chromatogram of Standard solution A, three bands are above and two bands are below the band of schisandrin. Standard solution B exhibits three bands in the middle-third section of the chromatogram, the most intense band with the highest Ris due to deoxyschisandrin. In the upper-third section of the chromatogram, Standard solution B exhibits two intense bands and one faint band, the most intense band corresponds to γ-schisandrin.

Acceptance criteria: Under UV light at 254 nm, the Sample solution chromatogram exhibits an intense band at an RF corresponding to the band due to schisandrin in the chromatogram of Standard solution A.  The Sample solution exhibits additional bands corresponding to similar bands in the chromatogram of Standard solution B. These include six bands in the lower-third section, three bands in the middle-third section, and two intense bands and one faint band in the upper-third section.

• C. HPLC

Analysis: Proceed as directed in the test for Content of Lignans.

Acceptance criteria: The chromatogram of Sampple solution is similar to the chromatogram of Standard solution B and the reference chromatogram provided with the lot of USP Schisandra chinensis Fruit Dry Extract RS. The chromatogram of the sample soution exhibits the peaks of schisandrin, schisandrol B, deoxyschisandrin, and γ-schisandrin with approximate relative retention times of 1.00, 1.29, 2.90 and 3.31, respectively. 

 

ASSAY

• Content of Lignans

 Solution A: Water

Solution B: A mixture of acetonitrile and methanol (1:1)

Mobile phase: See Table 1.

 

Table 1

 

Time (Min) Solution A (%) Solution B (%)
0 47 53
30 20 80

 

Solvent: Methanol

Standard solution A:  0.06 mg/mL of USP Schisandrin RS in Solvent

Standard solution B: 10 mg/mL of USP Schisandra chinensis Fruit Dry Extract RS in Solvent. Mix and pass through a polytetrafluoroethylene filter with pore size of 0.2 μm before injection.

Sample solution: Accurately transfer about 250 mg of Schisandra chinensis Fruit powder into a 50 mL centrifuge tube. Add 10 mL of methanol, and sonicate for 10 min (140 W, 42 kHz). Centrifuge, and transfer the supernatant to a 25 mL volumetric flask. Repeat the extraction one more time. Combine the supernatant to the 25 mL volumetric flask, adjust the solution with methanol to volume. Mix and pass through a polytetrafluoroethylene filter with pore size of 0.2 μm before injection, discard the first portion of the filtrate.

Chromatographic system

(See Chromatography <621>, System Suitability.)

Mode: UPLC

Detector: UV 251 nm

Column: 2.1 mm × 15 cm; 1.8-μm packing L1 (similar to ACQUITY UPLC® HSS Ts)

Column temperature: 353

Flow rate: 0.3 mL/min

Injection volume: 3 µL

System suitability

Sample: Standard solution A and Standard solution B

Suitability requirements

Chromatogram similarity: The chromatogram of Standard solution B is similar to the reference chromatogram provided with the lot of USP Schisandra chinensis Fruit Dry Extract RS being used

Tailing factor: NMT 2.0 for the peak of schisandrin in Standard solution A

Relative standard deviation: NMT 2.0% for schisandrin in Standard solution A

Resolution: NLT 1.5 between the peak of schisandrol B and the peak following it in Standard solution B

Analysis

Samples: Standard solution A, Standard solution B and Sample solution

Identify the the peaks of schisandrin, schisandrol B, deoxyschisandrin, and γ-schisandrin in Sample solution by comparison with the chromatogram of Standard solution A, Standard solution B and the reference chromatogram provided with the lot of USP Schisandra chinensis Fruit Dry Extract RS being used. The approximate relative retention times of the peaks mentioned above are 1.00, 1.29, 2.90, and 3.31 , respectively.

Calculate the percentage of lignans as the sum of schisandrin, schisandrol B, deoxyschisandrin, and γ-schisandrin in the portion of Schisandra chinensis Fruit Powder taken:

 

Result = (rU/rS) × CS × (V/W) × F × 100

 

rU   = peak area of relevant analyte from the Sample solution

rS   = perak area of schisandrin from Standard solution A

CS  = concentration of USP Schisandrin RS in Standard solution A (mg/mL)

V   = volume of the Sample solution (mL)

W   = weight of Schisandra chinensis Fruit taken to prepare the Sample solution (mg)

F = conversion factor for analytes (1.00 for schisandrin, 1.21 for schisandrol B, 1.00 for deoxyschisandrin, and 1.23 for γ-schisandrin)

 

 Acceptance criteria:

NLT 0.95% of the sum of schisandrin, schisandrol B, deoxyschisandrin and γ-schisandrin on the dried basis

 

CONTAMINANTS

• Articles of Botanical Origin, General Method for Pesticide Residues Analysis <561>: Meets the requirements

• Elemental Impurities—Procedures <233>

 Acceptance criteria

Arsenic: NMT 2.0 μg/g

Cadmium: NMT 0.3 µg/g

Lead: NMT 5.0 µg/g

Mercury: NMT 0.2 µg/g

• Microbial Enumeration Tests <2021>: 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.

• AbSence of Specified Microorganisms <2022>: Meets the requirements of the tests for the absence of Salmonella species and Escherichia coli

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

 

SPECIFIC TESTS

• Articles of Botanical Origin, Foreign Organic Matter <561>: NMT 1.0%

• Loss on Drying <731>

Analysis: Dry 2 g of Schisandra chinensis Fruit powder at 105° for 5 h

Acceptance criteria: NMT 16%

• Articles of Botanical Origin, Total Ash <561>

Analysis: 2 g of Schisandra chinensis Fruit powder

Acceptance criteria: NMT 7%

• Articles of Botanicle Origin, Water-Soluble Extractives <561>: Cold extraction method

Acceptance criteria: NMT 39%

• Articles of Botanical Origin, Total Alcohol-Soluble Extractives <561>: Cold extraction method

Acceptance criteria: NMT 40% 

 

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 of the plant contained in the article.

• USP Reference Standards <11>

USP Schisandra chinensis Fruit Dry Extract RS

USP Schisandrin RS

 

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Other Versions

Final Authorized Version 1.0
Proposed For Comment Version 0.2