Supplement I to the Japanese Pharmacopoeia Fourteenth Edition

1372 General Tests, Processes and Apparatus
Supplement I, JP XIV
Absorbance E 1z
1cm (245 nm): 473 – 502 (5 mg dried in a
desiccator (silica gel) for 24 hours, a mixture of methanol
and dilute acetic acid (7:3), 500 mL).
Purity Related substances—
(1) Dissolve 1.0 mg of rhynchophylline for component
determination in 1 mL of acetone, and perform the test with
this solution as directed under the Thin-layer Chromatography.
Spot 10 mL of the solution on a plate of silica
gel with ‰uorescent indicator for thin-layer chromatography,
develop with a mixture of 1-butanol, water and
acetic acid (100) (7:2:1) to a distance of about 10 cm, and
air-dry the plate. Examine under ultraviolet light (main
wavelength: 254 nm): any spot other than the principal spot
of Rf about 0.5 does not appear.
(2) Dissolve 5 mg of rhynchophylline for component determination
in 100 mL of a mixture of methanol and dilute
acetic acid (7:3), and use this solution as the sample solution.
Pipet 1 mL of the sample solution, add a mixture of
methanol and dilute acetic acid (7:3) to make exactly 100
mL, and use this solution as the standard solution. Perform
the test with exactly 20 mL each of the sample solution and
the standard solution as directed under the Liquid Chromatography
according to the following conditions. Determine
each peak area obtained from these solutions by the
automatic integration method: the sum of the peak areas except
the areas of rhynchophylline and the solvent obtained
from the sample solution is not more than the peak area of
rhynchophylline from the standard solution.
Operating conditions
Detector, column, column temperature, mobile phase,
and ‰ow rate: Proceed as directed in the operating conditions
in the Component determination under Uncaria
Thorn.
Time span of measurement: About 4 times as long as the
retention time of rhynchophylline after the solvent peak.
System suitability
Test for required detectability: Measure exactly 1 mL of
the standard solution, add a mixture of methanol and dilute
acetic acid (7:3) to make exactly 20 mL. Conˆrm that the
peak area of rhynchophylline obtained from 20 mL ofthis
solution is equivalent to 3.5 to 6.5z of that from 20 mL of
the standard solution.
System performance, and system repeatability: Proceed as
directed in the operating conditions in the Component determination
under Uncaria Thorn.
Sodium dihydrogen phosphate TS, pH 2.5 Dissolve 2.7
g of sodium dihydrogen phosphate dihydrate in 1000 mL of
water, and adjust the pH to 2.5 with phosphoric acid.
6 mol/L Sodium hydroxide TS Dissolve 252 g of sodium
hydroxide in water to make 1000 mL. Preserve in a polyethylene
bottle.
Sodium 1-methyl-1H-tetrazole-5-thiolate
C 2 H 3 N 4 NaS.2H 2 O White, crystals or crystalline powder.
Melting point: 90–949C
Purity Related substances—Dissolve 10 mg of sodium 1-
methyl-1H-tetrazole-5-thiolate in 10 mL of water, and use
this solution as the sample solution. Perform the test with
this solution as directed under the Thin-layer Chromatography.
Spot 5 mL of the sample solution on a plate of
silica gel with ‰uorescent indicator for thin-layer chromatography.
Develop the plate with a mixture of ethyl
acetate, acetone, water and acetic acid (100) (10:2:1:1) to a
distance of about 10 cm, and air-dry the plate. Examine under
ultraviolet light (main wavelength: 254 nm): any spot
other than the principal spot does not appear.
Sodium 2-naphthalenesulfonate C 10 H 7 NaO 3 S Pale
brown, crystals or powder.
Content: not less than 98.0z.
Sodium periodate TS Dissolve 60.0 g of sodium periodate
in 120 mL of 0.05 mol/L sulfuric acid TS, and add
water to make 1000 mL. If the solution is not clear, ˆlter this
through a glass-ˆlter. Keep in a light-resistant vessel.
Strongly acidic ion-exchange silica gel for liquid chromatography
Prepared for liquid chromatography.
Substrate solution for lysozyme hydrochloride To a suitable
amount of dried cells of Micrococcus luteus add a suitable
amount of phosphate buŠer solution, pH 6.2, gently
shake to make a suspension, and add the substrate cells or
the same buŠer solution so that the absorbance of the suspension
at 640 nm is about 0.65. Prepare before use.
Tetracycline Hydrochloride C 22 H 24 N 2 O 8 .HCl Yellow,
crystals or crystalline powder.
Purity Related substances—Dissolve 20 mg of tetracycline
hydrochloride in 25 mL of 0.01 mol/L hydrochloric
acid TS, and use this solution as the sample solution. Proceed
the test with 20 mL of the sample solution as directed in
the Purity (2) under Oxytetracycline Hydrochloride, determine
each peak area by the automatic integration method,
and calculate the amounts of them by the area percentage
method: the total amount of the peaks other than tetracycline
is not more than 10z.
Tetra‰uoroethylene polymer for gas chromatography
Prepared for gas chromatography.
Tetrahydrofuran for liquid chromatography C 4 H 8 O
Clear and colorless liquid.
Refractive index n 20
D : 1.406 – 1.409
Density (209C): 0.884 – 0.889 g/mL
Purity Ultraviolet absorbing substances—Determine the
absorption spectrum of tetrahydrofuran for liquid chromatography
as directed under the Ultraviolet-visible Spectrophotometry,
using water as the blank: the absorbences at
240 nm, 254 nm, 280 nm, 290 nm, and between 300 nm and
400 nm are not more than 0.35, 0.20, 0.05, 0.02 and 0.01, respectively.
Peroxide—Perform the test according to the method described
in JIS K 9705: not more than 0.01z.
Tetrakishydroxypropylethylenediamine for gas chromatography
Prepared for gas chromatography.