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shaolei1986

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[交流] 美国USP35文档求助，道客巴巴上的，有链接，谁帮忙下载下

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BRIEFING
Powdered Andrographis. A new USP Dietary Supplement monograph is proposed—
See briefing under Andrographis published elsewhere in this issue of PF.
(DSB: M. Sharaf.)
RTS—C66624
Add the following:

Powdered Andrographis
DEFINITION

Powdered Andrographis is Andrographis reduced to a fine or very fine powder.
IDENTIFICATION
•  A. THIN-LAYER CHROMATOGRAPHIC IDENTIFICATION TEST  201
Standard solution 1:  Use Standard solution A, prepared as directed in the test for
Content of Diterpene Lactones.
Standard solution 2:  Sonicate an amount of USP Powdered Andrographis Extract
RS, equivalent to about 15 mg of diterpene lactones, for 10–15 min in 25 mL of
methanol, centrifuge, and use the supernatant.
Sample solution:  Use Sample stock solution, prepared as directed in the test for
Content of Diterpene Lactones.
Adsorbent:  Chromatographic silica gel mixture with an average particle size of 10–15
µm (TLC plates)
Application volume:  10 µL, as 5–10 mm bands
Developing solvent system:  Chloroform, acetone, and toluene (2:2:1)
Spray reagent:  A mixture of 1% vanillin in alcohol and 10% sulfuric acid in alcohol
(1:1)
Analysis
Samples:  Standard solution 1, Standard solution 2, and Sample solution
Use a saturated chamber. Develop the chromatograms until the solvent front has
moved about 90% of the length of the plate. Remove the plate from the chamber,
dry, spray with the Spray reagent, heat for 5–10 min at 100 , and examine under
visible light.
Acceptance criteria:  The Sample solution exhibits three main grayish blue zones
with RF values of approximately 0.4, 0.6, and 0.8 that correspond in position and
color to the main zones of Standard solution 2. Standard solution 1 exhibits a grayish
blue zone due to andrographolide at an RF of about 0.4. The Sample solution
exhibits a zone similar in color and RF value to that due to andrographolide in
Standard solution 1.
•  B. The retention time of the main peak of the Sample solution obtained in the test for
Content of Diterpene Lactones corresponds to that of andrographolide in Standard
solution A. Identify other diterpene lactone peaks in the Sample solution by
comparison with Standard solution B and the reference chromatogram provided with
the lot of USP Powdered Andrographis Extract RS. The Sample solution shows
additional peaks corresponding to neoandrographolide, 14-deoxy-11,12-
didehydroandrographolide, and andrograpanin.
COMPOSITION
•  CONTENT OF DITERPENE LACTONES
Solution A:  Dissolve 0.14 g of potassium dihydrogen phosphate in 900 mL of water,
add 0.5 mL of phosphoric acid, dilute with water to 1000 mL, mix, filter, and degas.
Solution B:  Use filtered and degassed acetonitrile.
Standard solution A:  Dissolve a weighed quantity of USP Andrographolide RS in
methanol to obtain a solution having a known concentration of about 1.0 mg/mL.
Transfer 5.0 mL of this solution to a 10-mL volumetric flask, dilute with acetonitrile to
volume, and mix.
Standard solution B:  Transfer an amount of USP Powdered Andrographis Extract
RS, equivalent to about 25 mg of diterpene lactones, to a 50-mL volumetric flask,
add 25 mL of methanol, heat gently for 15–20 min, dilute with acetonitrile to volume,
and mix. Before injection, pass through a membrane filter having a 0.45-µm or finer
porosity, discarding the first 5 mL of the filtrate.
Sample stock solution:  Transfer about 2.0 g of Powdered Andrographis to a 250-mL
flask fitted with a reflux condenser. Add 50 mL of methanol, reflux on a water bath for
15 min, cool to room temperature, and decant the supernatant. Repeat until the last
extract is colorless. Combine the extracts, filter, concentrate under vacuum, and
adjust the volume to 50.0 mL using methanol. Transfer 25.0 mL of this solution to a
50-mL volumetric flask, dilute with acetonitrile to volume, and mix. Before injection,
pass through a membrane filter having a 0.45-µm or finer porosity, discarding the
first 5 mL of the filtrate.
Sample solution:  Transfer 25.0 mL of Sample stock solution to a 50-mL volumetric
flask, dilute with acetonitrile to volume, and mix. Before injection, pass through a
membrane filter having a 0.45-µm or finer porosity, discarding the first 5 mL of the
filtrate.
Mobile phase:  See the gradient table below.
Time (min) Solution A (%) Solution B (%)
0          95             5
18          55          45
25          20          80
28          20          80
35          55          45
40          95             5
45          95             5
Chromatographic system
(See Chromatography  621  , System Suitability.)
Mode:  LC
Detector:  UV 223 nm
Column:  4.6-mm × 25-cm; 5-µm packing L1
Flow rate:  1.5 mL/min
Injection size:  20 µL
System suitability
Samples:  Standard solution A and Standard solution B
Suitability requirements
[ NOTE— The chromatogram from Standard solution B is similar to the Reference
chromatogram provided with the lot of USP Powdered Andrographis Extract RS. ]
Column efficiency:  NLT 5000 theoretical plates, Standard solution A
Tailing factor:  NMT 1.5 for the andrographolide peak, Standard solution A
Relative standard deviation:  NMT 2.0%, determined from the andrographolide
peak for replicate injections, Standard solution A
Resolution:  NLT 5 between neoandrographolide and 14-deoxy-11,12-
didehydroandrographolide peaks, Standard solution B
Analysis
Samples:  Standard solution A, Standard solution B, and Sample solution
Using the chromatogram of Standard solution A, Standard solution B, and the
reference chromatogram provided with the lot of USP Powdered Andrographis
Extract RS, identify the retention times of the peaks corresponding to the different
diterpene lactones. The approximate relative retention times of the different
diterpene lactones are provided in the following table:
Analyte                         Relative Retention Time
Andrographolide                                  1.00
Neoandrographolide                               1.16
14-Deoxy-11,12-didehydroandrographolide             1.31
Andrograpanin                                     1.50
Separately calculate the percentages of andrographolide, neoandrographolide, 14-
deoxy-11,12-didehydroandrographolide, and andrograpanin in the portion of
Powdered Andrographis taken:
Result = 10(CS /W)(rU /rS ) × F
rU  = peak response for each diterpene lactone from the Sample solution
rS  = peak response for andrographolide from Standard solution A
CS = concentration of USP Andrographolide RS in the Standard solution A
(mg/mL)
W = weight of Powdered Andrographis taken to prepare the Sample solution (g)
F = conversion factor for each analyte (1.00 for andrographolide, 3.90 for
neoandrographolide, 1.45 for 14-deoxy-11,12-didehydroandrographolide, and
2.65 for andrograpanin)
Acceptance criteria:  NLT 1.0%, on the dried basis, of the sum of the percentages of
andrographolide, neoandrographolide, 14-deoxy-11,12-didehydroandrographolide,
and andrograpanin
IMPURITIES
Inorganic Impurities
• ARTICLES OF BOTANICAL ORIGIN, Acid-Insoluble Ash  561  : NMT 3.0%
• HEAVY METALS, Method II 231  : NMT 20 ppm
Organic Impurities
•  PROCEDURE: ARTICLES OF BOTANICAL ORIGIN, General Method for Pesticide Residues
Analysis  561  : Meets the requirements
SPECIFIC TESTS
•  BOTANIC CHARACTERISTICS
Macroscopic:  It is a grayish brown powder.
Histology
Microscopic examination:  It reveals cells of the upper and lower epidermis of the
leaves, some cells containing large cystoliths, up to 36 µm in diameter and 180 µm
long, with a hilum-shaped scar in the large end; 1–4 celled nonglandular hairs;
disk-shaped glandular hairs, 8-celled head and very short stalk; diacytic stomata
mostly on the lower epidermis; stem epidermal cells, some cells containing
cystoliths, stomata, nonglandular hairs and glandular hairs similar to those of the
leaves; thin-walled parenchyma cells; collenchyma cells; acicular phloem fibers;
tracheids; vessels, with spiral and scalariform thickening.
• LOSS ON DRYING  731  : Dry 1.0 g of finely Powdered Andrographis at 105  for 3 h: it loses NMT 12.0% of its weight.
• ARTICLES OF BOTANICAL ORIGIN, Total Ash  561  : NMT 15%, determined on 1.0 g of finely Powdered Andrographis
• ARTICLES OF BOTANICAL ORIGIN, Alcohol-Soluble Extractives, Method 2  561  : NLT 8.0%
• MICROBIAL ENUMERATION TESTS—NUTRITIONAL AND DIETARY SUPPLEMENTS  2021  : The total aerobic bacterial count does not exceed 105 cfu/g; the total combined moldsand 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—NUTRITIONAL AND DIETARY SUPPLEMENTS 2022  : Meets the requirements of the tests for absence of Salmonella species and Escherichia coli
ADDITIONAL REQUIREMENTS
•  PACKAGING AND STORAGE: Preserve in well-closed containers, protected from light andmoisture, and store at room temperature.
•  LABELING: The label states the Latin binomial and, following the official name, the parts of the plant contained in the article.
• USP REFERENCE STANDARDS  11
USP Andrographolide RS
USP Powdered Andrographis Extract RS  2S (USP33)