奥氮平片美国药典36版质量标准USP36

4562Olanzapine / Official Monographs USP 36

C U= concentration of Olanzapine in the Sample C U= concentration of Olanzapine in the Sample

solution (mg/mL)solution (mg/mL)

Acceptance criteria:98.0%–102.0% on the anhydrous,F= relative response factor for each impurity from solvent-free basis Table 2

Acceptance criteria:See Table 2.

IMPURITIES

•R ESIDUE ON I GNITION〈281〉:NMT 0.1%

Table 2

•H EAVY M ETALS, Method II〈231〉:NMT 10ppm

Relative Relative Acceptance

Retention Response Criteria, Change to read:Name Time Factor NMT (%)

Olanzapine related

•O RGANIC I MPURITIES compound B

a0.3 2.30.10 Buffer:Dissolve 13g of sodium dodecyl sulfate in

Olanzapine related

1500mL of water. Add 5mL of phosphoric acid, and

compound A b0.8v2.3v USP360.10 adjust with a sodium hydroxide solution to a pH of 2.5.

Olanzapine 1.0——Solution A:Acetonitrile and Buffer (48:52)

Solution B:Acetonitrile and Buffer (70:30)•Chloromethyl

Mobile phase:See Table 1.olanzapinium

chloride c (if pres-0.15•(RB 1-Jun-

ent) 1.1 1.02012)

Table 1

Any individual, un-

——Time Solution A Solution B specified impurity0.10

(min)(%)(%)

Total impurities——0.4 01000

a2-Methyl-10H-thieno-[2,3-b][1,5]benzodiazepin-4[5H]-one.

101000

b5-Methyl-2-((2-nitrophenyl)amino)-3-thiophenecarbonitrile.

200100•c1-Chloromethyl-1-methyl-4-(2-methyl-10H-benzo[b]thieno[2,3-e][1,

2501004]diazepin-4-yl)piperazin-1-ium chloride.•(RB 1-Jun-2012)

271000SPECIFIC TESTS

351000•W ATER D ETERMINATION, Method I〈921〉

[N OTE—A suitable solvent system for water determina-Edetate disodium solution:37mg/L of edetate diso-tion in ketones and aldehydes (e.g., Hydranal compos-

dium in Buffer ite 5K-working medium K or Aquastar composite 5K-Diluent:Acetonitrile and Edetate disodium solution solvent KC or equivalent) is recommended.]

(40:60)Acceptance criteria:NMT 1.0%

System suitability solution:20µg/mL of USP

Olanzapine RS and 2µg/mL each of USP Olanzapine ADDITIONAL REQUIREMENTS

Related Compound A RS and USP Olanzapine Related•P ACKAGING AND S TORAGE:Preserve in well-closed contain-Compound B RS in Diluent ers, and store at room temperature.

Standard solution:2µg/mL of USP Olanzapine RS in•USP R EFERENCE S TANDARDS〈11〉

Diluent USP Olanzapine RS

Sample solution:0.4mg/mL of Olanzapine in Diluent USP Olanzapine Related Compound A RS

Chromatographic system5-Methyl-2-((2-nitrophenyl)amino)-

(See Chromatography 〈621〉, System Suitability.)3-thiophenecarbonitrile.

Mode:LC C

12H9N3O2S259.28

Detector:UV 220 nm USP Olanzapine Related Compound B RS

Column:4.6-mm × 25-cm; 5-µm packing L72-Methyl-10H-thieno-[2,3-b][1,5]benzodiazepin-4[5H]-Temperatures one.

Column:35°C

12H10N2OS230.29

Sample:5°

Flow rate:1.5mL/min

Injection volume:20µL

System suitability

Sample:System suitability solution Olanzapine Tablets

[N OTE—Identify the peaks using the Relative Retention

Time values given in Table 2.]DEFINITION

Suitability requirements Olanzapine Tablets contain NLT 90.0% and NMT 110.0% Resolution:NLT 3.0 between olanzapine related com-of the labeled amount of olanzapine (C

17H20N4S).

pound A and olanzapine

Tailing factor:NMT 1.5 for the olanzapine peak IDENTIFICATION

Relative standard deviation:NMT 2.0% from four

replicate injections for the olanzapine peak

Change to read:

Analysis

Samples:Standard solution and Sample solution

•I NFRARED A BSORPTION〈197S〉

Calculate the percentage of each impurity in the portion

Standard solution:v30v USP36 mg/mL of USP Olanzapine of Olanzapine taken:

RS in chloroform

Result = (r U/r S) × (C S/C U) × (1/F) × 100Sample solution:Dissolve a quantity of powdered Tab-

lets, equivalent to 30mg of olanzapine, in 30mL of r U= peak response of each impurity from the chloroform, and filter. Evaporate completely to dryness Sample solution with the aid of a current of air. Redissolve the residue in r S= peak response of olanzapine from the1mL of chloroform.

Standard solution

C S= concentration of USP Olanzapine RS in the

Standard solution (mg/mL)