Supplement II, JP XVII O‹cial Monographs 2955

Assay Pipet a volume of Ritodrine Hydrochloride Injec-

tion, equivalent to about 20 mg of ritodrine hydrochloride Saccharin
(C17H21NO3.HCl), and add a mixture of 0.02 mol/L sodium
dihydrogen phosphate dihydrate solution and methanol サッカリン
(7:3) to make exactly 250 mL, and use this solution as the
sample solution. Separately, weigh accurately about 20 mg Delete the description of harmonization in the
of Ritodrine Hydrochloride RS, previously dried at 1059C beginning and symbols ( ◆ ◆) in the Descrip-
for 2 hours, dissolve in a mixture of 0.02 mol/L sodium di- tion, Melting point, Purity (2) and (4), and Con-
hydrogen phosphate dihydrate solution and methanol (7:3) tainers and storage.
to make exactly 250 mL, and use this solution as the stand-
ard solution. Perform the test with exactly 10 mL each of the
sample solution and standard solution as directed under Saccharin Sodium Hydrate
Liquid Chromatography <2.01> according to the following
conditions. Determine the peak areas, AT and AS, of rito- サッカリンナトリウム水和物
drine in each solution.
Delete the description of harmonization in the
Amount (mg) of ritodrine hydrochloride (C17H21NO3.HCl)
beginning and symbols ( ◆ ◆) in the Descrip-
＝ M S × AT / AS
tion, Purity (3) and (5), and Containers and
MS: Amount (mg) of Ritodrine Hydrochloride RS taken storage.
Operating conditions—
Detector: An ultraviolet absorption photometer (wave-
length: 220 nm). Light Anhydrous Silicic Acid
Column: A stainless steel column 6 mm in inside diameter
軽質無水ケイ酸
and 15 cm in length, packed with octylsilanized silica gel for
liquid chromatography (5 mm in particle diameter).
Delete the Volume test:
Column temperature: A constant temperature of about
259C.
Mobile phase: Dissolve 6.6 g of diammonium hydrogen
Add the following:
phosphate and 1.1 g of sodium 1-heptansulfonate in 840 mL
of water, add 160 mL of acetonitrile for liquid chromatog-
raphy, and adjust to pH 3.0 with phosphoric acid. Sitagliptin Phosphate Hydrate
Flow rate: Adjust so that the retention time of ritodrine is
シタグリプチンリン酸塩水和物
about 19 minutes.
System Suitability—
System performance: Dissolve 10 mg of ritodrine hydro-
chloride in 50 mL of dilute sulfuric acid. Heat a portion of
this solution in a water bath for about 30 minutes, and
allow to cool. Measure a portion of this solution, and add
the same volume of 2 mol/L sodium hydroxide TS. Dissolve
2 mg of ritodrine hydrochloride in 10 mL of this solution,
C16H15F6N5O.H3PO4.H2O: 523.32
and add a mixture of 0.02 mol/L sodium dihydrogen phos-
(3R)-3-Amino-1-[3-(tri‰uoromethyl)-5,6-
phate dihydrate solution and methanol (7:3) to make 25
dihydro[1,2,4]triazolo[4,3-a]pyrazin-7(8H)-yl]-4-(2,4,5-
mL. When the procedure is run with 10 mL of this solution
tri‰uorophenyl)butan-1-one monophosphate monohydrate
under the above operating conditions, ritodrine and rito-
[654671-77-9]
drine threo-isomer are eluted in this order with the resolu-
tion between these peaks being not less than 3.
Sitagliptin Phosphate Hydrate contains not less
System repeatability: When the test is repeated 6 times
than 98.0z and not more than 102.0z of sitagliptin
with 10 mL of the standard solution under the above operat-
phosphate (C16H15F6N5O.H3PO4: 505.31), calculated
ing conditions, the relative standard deviation of the peak
on the anhydrous basis.
area of ritodrine is not more than 1.0z.
Description Sitagliptin Phosphate Hydrate occurs as a
Containers and storage Containers—Hermetic containers.
white powder.
Storage—At a temperature between 29C and 89C.
It is soluble in water, sparingly soluble in methanol, very
slightly soluble in acetonitrile and in ethanol (99.5).

Identiˆcation (1) Determine the absorption spectrum of

a solution of Sitagliptin Phosphate Hydrate (1 in 10,000)
as directed under Ultraviolet-visible Spectrophotometry

The JP Drugs are to be tested according to the provisions given in the pertinent monographs, General Notices, General Rules for Crude Drugs,
General Rules for Preparations, and General Tests for their conformity to the Japanese Pharmacopoeia. (See the General Notices 5.)