Zolpidem Tartrate Extended-Release Tablets
DEFINITION
Zolpidem Tartrate Extended-Release Tablets contain NLT 90.0% and NMT 110.0% of the labeled amount of zolpidem tartrate (C42H48N6O8).
IDENTIFICATION
• A. Ultraviolet Absorption 197U
Sample:
25 µg/mL of zolpidem tartrate in 0.01 M hydrochloric acid from a suitable quantity of powder obtained by grinding 1 Tablet
• B.
The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.
ASSAY
• Procedure
Buffer:
3.3 mL of phosphoric acid in 1 L of water. Adjust with triethylamine to a pH of 5.5.
Mobile phase:
Acetonitrile, methanol, and Buffer (4:5:11)
Standard stock solution:
0.5 mg/mL of USP Zolpidem Tartrate RS in a mixture of alcohol and 0.01 M hydrochloric acid (4:1)
Standard solution:
0.1 mg/mL of USP Zolpidem Tartrate RS in Mobile phase from the Standard stock solution
Sample stock solution:
Finely powder NLT 8 Tablets. Transfer the powder quantitatively to a suitable volumetric flask to obtain 0.5 mg/mL of zolpidem tartrate. Add 70% of the flask volume of a mixture of alcohol and 0.01 M hydrochloric acid (5:2), and stir on a magnetic stirrer for 1 h. Dilute with alcohol to volume. Allow solid particles to settle, and pass the supernatant through a suitable filter (Whatman 40 or equivalent).
Sample solution:
0.1 mg/mL of zolpidem tartrate from filtered Sample stock solution in Mobile phase
Chromatographic system
Mode:
LC
Detector:
UV 240 nm
Column:
4.6-mm × 15-cm; 5-µm packing L1
Column temperature:
40
Flow rate:
1 mL/min
Injection size:
15 µL
System suitability
Sample:
Standard solution
Suitability requirements
Tailing factor:
NMT 3.0 for zolpidem
Relative standard deviation:
NMT 2.0% for zolpidem
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of the labeled amount of zolpidem tartrate (C42H48N6O8) in the portion of Tablets taken:
Result = (rU/rS) × (CS/CU) × 100
Acceptance criteria:
90.0%110.0%
PERFORMANCE TESTS
Change to read:
• Dissolution 711
Test 1(RB 1-Jul-2011)
Medium:
0.01 N hydrochloric acid; 500 mL
Apparatus 1:
100 rpm
Times:
30, 90, and 240 min
Standard solution:
Solution of USP Zolpidem Tartrate RS in Medium containing (L/500) mg/mL, where L is the label claim in mg/Tablet
Sample solution:
Pass a portion of the solution under test through a suitable filter.
Detector:
UV 295 nm
Cell path:
1 cm
Blank:
Medium
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of the labeled amount of zolpidem tartrate (C42H48N6O8) dissolved:
Result = (AU/AS) × (CS/L) × V × 100
Tolerances:
See Table 1.
Table 1
The percentages of the labeled amount of zolpidem tartrate (C42H48N6O8) dissolved in the times specified conform to Acceptance Table 2 in Dissolution 711.
Test 2:
If the product complies with this test, the labeling indicates that it meets USP Dissolution Test 2.
Medium, Apparatus, and Times:
Proceed as directed for Test 1.
Standard solution:
Solution of USP Zolpidem Tartrate RS in Medium containing (L/500) mg/mL, where L is the label claim in mg/Tablet
Sample solution:
Pass a portion of the solution under test through a suitable filter.
Detector:
UV 295 nm
Blank:
Medium
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of the labeled amount of zolpidem tartrate (C42H48N6O8) dissolved:
Result = (AU/AS) × (CS/L) × V × 100
Tolerances:
See Table 2.
Table 2
The percentages of the labeled amount of zolpidem tartrate (C42H48N6O8) dissolved in the times specified conform to Acceptance Table 2 in Dissolution 711.
Test 3:
If the product complies with this test, the labeling indicates that it meets USP Dissolution Test 3.
Medium:
0.01 N hydrochloric acid; 500 mL
Apparatus 1:
100 rpm
Times:
30, 90, and 120 min
Standard solution:
Solution of USP Zolpidem Tartrate RS in Medium containing (L/500) mg/mL, where L is the label claim in mg/Tablet
Sample solution:
Pass a portion of the solution under test through a suitable filter.
Detector:
UV 237 nm
Blank:
Medium
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of the labeled amount of zolpidem tartrate (C42H48N6O8) dissolved:
Result = (AU/AS) × (CS/L) × V × 100
Tolerances:
See Table 3.
Table 3
The percentages of the labeled amount of zolpidem tartrate (C42H48N6O8) dissolved in the times specified conform to Acceptance Table 2 in Dissolution 711.(RB 1-Jul-2011)
• Uniformity of Dosage Units 905:
Meet the requirements
IMPURITIES
Change to read:
• Organic Impurities
Buffer, Mobile phase, Standard stock solution, Sample solution, and Chromatographic system:
Proceed as directed in the Assay.
System suitability solution:
Dissolve a suitable amount of USP Zolpidem Related Compound A RS in Standard stock solution to obtain a solution containing 1 µg/mL of zolpidem related compound A. Dilute 1 mL of the resulting solution with Mobile phase to 5 mL.
System suitability
Sample:
System suitability solution
Suitability requirements
Resolution:
NLT 1.5 between zolpidem related compound A and zolpidem
Tailing factor:
NMT 3.0 for the zolpidem peak
Relative standard deviation:
NMT 2.0% for the zolpidem peak
Analysis
Sample:
Sample solution
Calculate the percentage of each impurity in the portion of Tablets taken:
Result = (rU/rT) × (1/F) × 100
Acceptance criteria:
See Table 4.
Table 4
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in well-closed containers, and store at controlled room temperature.
Add the following:
• Labeling:
When more than one Dissolution test is given, the labeling states the Dissolution test used only if Test 1 is not used.(RB 1-Jul-2011)
• USP Reference Standards 11
USP Zolpidem Related Compound A RS
N,N-Dimethyl-2-(7-methyl-2-p-tolylimidazo[1,2-a]pyridin-3-yl)acetamide. C19H21N3O 307.39
Auxiliary Information
Please check for your question in the FAQs before contacting USP.
USP35NF30 Page 5084
Pharmacopeial Forum: Volume No. 35(3) Page 595
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