Supplement I to the Japanese Pharmacopoeia Fourteenth Edition

1384 O‹cial Monographs for Part I
Supplement I, JP XIV
Standard
Internal standard solution—A solution of guaifenesin in the
mobile phase (1 in 200).
Operating conditions—
Detector: An ultraviolet absorption photometer (wavelength:
230 nm).
Column: A stainless steel column 4.6 mm in inside diameter
and 15 cm in length, packed with octadecylsilanized
silica gel for liquid chromatography (5 mm in particle
diameter).
Column temperature: A constant temperature of about
259C.
Mobile phase: Dissolve 5.94 g of diammonium hydrogen
phosphate in 850 mL of water, add 100 mL of acetonitrile,
adjust the pH to 5.0 with phosphoric acid, and add water to
make exactly 1000 mL.
Flow rate: Adjust the ‰ow rate so that the retention time
of ampicillin is about 6 minutes.
System suitability—
System performance: When the procedure is run with
10 mL of the standard solution under the above operating
conditions, ampicillin and the internal standard are eluted in
this order with the resolution between these peaks being not
less than 40.
System repeatability: When the test is repeated 6 times
with 10 mL of the standard solution under the above operating
conditions, the relative standard deviation of the ratios
of the peak area of ampicillin to that of the internal standard
is not more than 1.0z.
Containers and storage
Anhydrous Ampicillin
無 水 アンピシリン
Containers—Tight containers.
Change to read except the structural formula
and chemical name:
Anhydrous Ampicillin contains not less than 960 mg
(potency) per mg, calculated on the anhydrous basis.
The potency of Anhydrous Ampicillin is expressed as
mass (potency) of ampicillin (C 16 H 19 N 3 O 4 S).
Description Anhydrous Ampicillin occurs as white to light
yellowish white, crystals or crystalline powder. It is sparingly
soluble in water, slightly soluble in methanol, very slightly
soluble in ethanol (95), and practically insoluble in acetonitrile.
Identiˆcation Determine the infrared absorption spectrum
of Anhydrous Ampicillin as directed in the potassium
bromide disk method under the Infrared Spectrophotometry,
and compare the spectrum with the Reference Spectrum:
both spectra exhibit similar intensities of absorption at the
same wave numbers.
the
Optical rotation [a] 20
D : +280 – +3059(0.5 g calculated on
anhydrous basis, water, 100 mL, 100 mm).
pH The pH of a solution obtained by dissolving 1.0 g of
Anhydrous Ampicillin in 100 mL of water is between 4.0 and
5.5.
Purity (1) Heavy metals—Proceed with 1.0 g of Anhydrous
Ampicillin according to Method 2, and perform the
test. Prepare the control solution with 2.0 mL of Standard
Lead Solution (not more than 20 ppm).
(2) Arsenic—Prepare the test solution with 1.0 g of Anhydrous
Ampicillin according to Method 3, and perform the
test (not more than 2 ppm).
(3) Related substances—Dissolve 0.05 g of Anhydrous
Ampicillin in the mobile phase to make 50 mL, and use this
solution as the sample solution. Pipet 1 mL of the sample
solution, add the mobile phase to make exactly 100 mL, and
use this solution as the standard solution. Perform the test
with exactly 10 mL each of the sample solution and the standard
solution as directed under the Liquid Chromatography
according to the following conditions, and determine each
peak area by the automatic integration method: the area of
each peak other than ampicillin from the sample solution is
not more than the peak area of ampicillin from the standard
solution.
Operating conditions—
Detector, column, column temperature, mobile phase,
and ‰ow rate: Proceed as directed in the operating conditions
in the Assay.
Time span of measurement: As long as about 10 times of
the retention time of ampicillin.
System suitability—
Test for required detectability: To exactly 1 mL of the
standard solution add the mobile phase to make exactly
10 mL. Conˆrm that the peak area of ampicillin obtained
from 10 mL of this solution is equivalent to 7 to 13z of that
from 10 mL of the standard solution.
System performance, and system repeatability: Proceed as
directed in the system suitability in the Assay.
Water Not more than 2.0z (2.5 g, volumetric titration,
direct titration).
Assay Weigh accurately an amount of Anhydrous Ampicillin
and Ampicillin Reference Standard, equivalent to
about 50 mg (potency), add exactly 5 mL each of the internal
standard solution and the mobile phase to make 50 mL, and
use these solutions as the sample solution and the standard
solution. Perform the test with 10 mL eachofthesample
solution and the standard solution as directed under the
Liquid Chromatography according to the following conditions,
and determine the ratios, Q T and Q S , of the peak area
of ampicillin to that of the internal standard.
Amount [mg (potency)] of ampicillin (C 16 H 19 N 3 O 4 S)
= W S × Q T
Q S
× 1000
W S : Amount [mg (potency)] of Ampicillin Reference
Standard
Internal standard solution—A solution of guaifenesin in the