JP XVIII Official Monographs / Pentobarbital Calcium 1491

the plate. Allow to stand for 5 minutes in iodine vapor: any

Pentazocine spot other than the principal spot obtained from the sample
solution is not more intense than the spot from the standard
ペンタゾシン solution.
Loss on drying <2.41> Not more than 0.5z (1 g, in vacu-
C, 5 hours).
um, phosphorus (V) oxide, 609
Residue on ignition <2.44> Not more than 0.2z (1 g).
Assay Weigh accurately about 0.5 g of Pentazocine, previ-
ously dried, dissolve in 50 mL of acetic acid (100), and titrate
<2.50> with 0.1 mol/L perchloric acid VS (indicator: 2 drops
of crystal violet TS). Perform a blank determination in the
same manner, and make any necessary correction.
C19H27NO: 285.42
Each mL of 0.1 mol/L perchloric acid VS
(2RS,6RS,11RS )-6,11-Dimethyl-
＝ 28.54 mg of C19H27NO
3-(3-methylbut-2-en-1-yl)-1,2,3,4,5,6-hexahydro-
2,6-methano-3-benzoazocin-8-ol Containers and storage Containers—Well-closed contain-
[359-83-1] ers.

Pentazocine, when dried, contains not less than

99.0z of pentazocine (C19H27NO). Pentobarbital Calcium
Description Pentazocine occurs as a white to pale yellow-
ペントバルビタールカルシウム
white, crystalline powder. It is odorless.
It is freely soluble in acetic acid (100) and in chloroform,
soluble in ethanol (95), sparingly soluble in diethyl ether and
practically insoluble in water.
Identification (1) To 1 mg of Pentazocine add 0.5 mL of
formaldehyde-sulfuric acid TS: a deep red color is produced,
and it changes to grayish brown immediately.
(2) Dissolve 5 mg of Pentazocine in 5 mL of sulfuric C22H34CaN4O6: 490.61
acid, add 1 drop of iron (III) chloride TS, and heat in a Monocalcium bis[5-ethyl-5-[(1RS )-1-methylbutyl]-4,6-
water bath for 2 minutes: the color of the solution changes dioxo-1,4,5,6-tetrahydropyrimidin-2-olate]
from light yellow to deep yellow. Shake the solution with 1 [76-74-4, Pentobarbital]
drop of nitric acid: the solution remains yellow in color.
(3) Determine the absorption spectrum of a solution of Pentobarbital Calcium contains not less than 98.0z
Pentazocine in 0.01 mol/L hydrochloric acid TS (1 in and not more than 102.0z of pentobarbital calcium
10,000) as directed under Ultraviolet-visible Spectropho- (C22H34CaN4O6), calculated on the dried basis.
tometry <2.24>, and compare the spectrum with the Refer-
Description Pentobarbital Calcium occurs as a white pow-
ence Spectrum: both spectra exhibit similar intensities of ab-
der.
sorption at the same wavelengths.
It is sparingly soluble in water, slightly soluble in ethanol
Absorbance <2.24> E 11zcm (278 nm): 67.5 – 71.5 (after dry- (95), and practically insoluble in acetonitrile.
ing, 0.1 g, 0.01 mol/L hydrochloric acid TS, 1000 mL). A solution of Pentobarbital Calcium (1 in 100) shows no
optical rotation.
Melting point <2.60> 150 – 1589C
Identification (1) Determine the infrared absorption spec-
Purity (1) Clarity and color of solution—Dissolve 0.10 g
trum of Pentobarbital Calcium as directed in the potassium
of Pentazocine in 20 mL of 0.1 mol/L hydrochloric acid TS:
bromide disk method under Infrared Spectrophotometry
the solution is clear and colorless.
<2.25>, and compare the spectrum with the Reference Spec-
(2) Heavy metals <1.07>—Proceed with 1.0 g of Pentazo-
trum: both spectra exhibit similar intensities of absorption at
cine according to Method 2, and perform the test. Prepare
the same wave numbers.
the control solution with 2.0 mL of Standard Lead Solution
(2) To 1 g of Pentobarbital Calcium add 5 mL of ethanol
(not more than 20 ppm).
(95) and 5 mL of dilute hydrochloric acid, dissolve by warm-
(3) Arsenic <1.11>—Prepare the test solution with 1.0 g
ing with shaking, shake with 5 mL of dilute hydrochloric
of Pentazocine according to Method 3, and perform the test
acid and 10 mL of water, allow to cool, and filter. To the fil-
with a solution of magnesium nitrate hexahydrate in ethanol
trate add 1 drop of methyl red TS, and add ammonia TS
(95) (1 in 10) (not more than 2 ppm).
until a slight yellow color develops: the solution responds to
(4) Related substances—Dissolve 0.20 g of Pentazocine
Qualitative Tests <1.09> (1), (2) and (3) for calcium salt.
in 10 mL of chloroform, and use this solution as the sample
solution. Pipet 1 mL of the sample solution, add chloroform Purity (1) Chloride <1.03>—To 1.0 g of Pentobarbital
to make exactly 100 mL, and use this solution as the stand- Calcium add 5 mL of ethanol (95) and 2.5 mL of dilute nitric
ard solution. Perform the test with these solutions as di- acid, dissolve by warming with shaking, cool, add water to
rected under Thin-layer Chromatography <2.03>. Spot 10 mL make 50 mL, shake well, and filter. Discard the first 10 mL
each of the sample solution and standard solution on a plate of the filtrate, and to 15 mL of the subsequent filtrate add 6
of silica gel for thin-layer chromatography. Develop the mL of dilute nitric acid and water to make 50 mL. Perform
plate with a mixture of chloroform, methanol and isopro- the test using this solution as the test solution. Prepare the
pylamine (94:3:3) to a distance of about 13 cm, and air-dry control solution as follows: To 0.30 mL of 0.01 mol/L hy-

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.)