Nateglinide Tablets
DEFINITION
Nateglinide Tablets contain NLT 95.0% and NMT 105.0% of the labeled amount of nateglinide (C19H27NO3).
IDENTIFICATION
•  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
Diluent:  Acetonitrile and water (11:9)
Mobile phase:  Acetonitrile and 0.05% solution of trifluoroacetic acid (23:27)
Standard solution:  0.72 mg/mL of USP Nateglinide RS prepared as follows. Transfer USP Nateglinide RS to a suitable volumetric flask, and add acetonitrile to 40% of the volume of the flask. [Note—Sonicate to dissolve. ] Add water equivalent to 30% of the final volume, mix, cool the solution to room temperature, and dilute with Diluent to volume.
Sample solution:  Place 20 Tablets into a 500-mL volumetric flask, and add 60 mL of water to disintegrate the Tablets. [Note—Sonicate with cooling, if necessary. ] Add 280 mL of acetonitrile, and shake by mechanical means for at least 30 min. Dilute with Diluent to volume. Pass a portion through a 0.45-µm glass microfiber filter, discarding the first 10 mL of the filtrate, or use centrifugation to obtain a clear solution. Dilute an aliquot of this solution with Diluent to obtain a solution having a concentration of 0.72 mg/mL based on the label claim.
Chromatographic system 
Mode:  LC
Detector:  UV 210 nm
Column:  4.6-mm × 15-cm; 5-µm packing L1
Flow rate:  1.5 mL/min
Injection size:  10 µL
System suitability 
Sample:  Standard solution
Suitability requirements 
Tailing factor:  NMT 1.8
Relative standard deviation:  NMT 2.0%
Analysis 
Samples:  Standard solution and Sample solution
Calculate the percentage of the labeled quantity of C19H27NO3 in the portion of Tablets taken:
Result = (rU/rS) × (CS/CU) × 100
rU== peak response from the Sample solution
rS== peak response from the Standard solution
CS== concentration of the Standard solution (mg/mL)
CU== nominal concentration of the Sample solution (mg/mL)
Acceptance criteria:  95.0%–105.0%
PERFORMANCE TESTS
•  Dissolution 711
Medium:  0.01 N hydrochloric acid containing 0.5% (w/v) of sodium lauryl sulfate; 1000 mL
Apparatus 2:  50 rpm
Time:  30 min
Determine the quantity of C19H27NO3 dissolved by employing the following method.
Solution A:  6.9 mg/mL of monobasic sodium phosphate. Adjust with phosphoric acid to a pH of 2.5.
Mobile phase:  Acetonitrile and Solution A (45:55)
Standard stock solution:  0.3 mg/mL of USP Nateglinide RS prepared as follows. Transfer USP Nateglinide RS to a suitable volumetric flask, dissolve in a small volume of acetonitrile not exceeding 5% of the final volume, and dilute with Medium to volume.
Standard solution:  0.12 mg/mL of USP Nateglinide RS in Medium, from the Standard stock solution
Sample solution:  Pass through a suitable filter with pore size of 0.7 µm.
Chromatographic system 
Mode:  LC
Detector:  UV 210 nm
Column:  4.6-mm × 5-cm; 5-µm packing L1
Flow rate:  1.5 mL/min
Injection size:  10 µL
System suitability 
Sample:  Standard solution
Suitability requirements 
Tailing factor:  NMT 2.0
Relative standard deviation:  NMT 2.0%
Analysis 
Samples:  Standard solution and Sample solution
Calculate the percentage of C19H27NO3 dissolved:
Result = (rU/rS) × (CS × V) × (100/L)
rU== peak response from the Sample solution
rS== peak response from the Standard solution
CS== concentration of the Standard solution (mg/mL)
V== volume of Medium, 1000 mL
L == label claim (mg/Tablet)
Tolerances:  NLT 80% (Q) of the labeled amount of C19H27NO3 is dissolved.
•  Uniformity of Dosage Units 905: Meet the requirements
ADDITIONAL REQUIREMENTS
•  Packaging and Storage: Preserve in tight containers, and store at controlled room temperature.
•  USP Reference Standards 11
USP Nateglinide RS Click to View Structure
Auxiliary Information— Please check for your question in the FAQs before contacting USP.
Topic/Question Contact Expert Committee
Monograph Elena Gonikberg, Ph.D.
Principal Scientific Liaison
1-301-816-8251
(SM32010) Monographs - Small Molecules 3
711 Margareth R.C. Marques, Ph.D.
Senior Scientific Liaison
1-301-816-8106
(GCDF2010) General Chapters - Dosage Forms
Reference Standards RS Technical Services
1-301-816-8129
rstech@usp.org
USP35–NF30 Page 4006
Pharmacopeial Forum: Volume No. 35(2) Page 281