Кеторолак, раствор для инъекций

[Dashkevich_ns]

Необходимо определить кеторолак и родственные примеси в растворе для инъекций, подобрать методику, условия проведения эксперимента? Метод определения -  ВЭЖХ. Если есть у кого-то статьи, работы по этой теме, буду рада, если поделитесь

[Arkadiy]

Для ВЭЖХ. нужен стандартные образцы субстанции и родственных примесей. Они у вас есть?

[-omicronic-]

Ketorolac Tromethamine Injection

 

DEFINITION

Ketorolac Tromethamine Injection is a sterile solution of Ketorolac Tromethamine. It contains NLT 90.0% and NMT 110.0% of the labeled amount of ketorolactromethamine (C15H13NO3 · C4H11NO3 ).

IDENTIFICATION

•  A.

Sample:  Standard solution and Sample solution (1:1), prepared as directed in the Assay

Analysis:  Chromatograph the Sample as directed in the Assay.

Acceptance criteria:  The chromatogram obtained exhibits two main peaks corresponding to ketorolac and the internal standard.

ASSAY

•  Procedure

[NOTE— Protect all the solutions from light. ]

Mobile phase:  Methanol, water, and glacial acetic acid (55:44:1)

Diluent:  Methanol and water (1:1). [NOTE— Resolution may be increased by increasing the proportion of water in the Mobile phase. ]

Internal standard solution:  0.3 mg/mL of naproxen in methanol

Standard stock solution:  0.24 mg/mL of USP Ketorolac Tromethamine RS in methanol

Standard solution:  0.024 mg/mL of USP Ketorolac Tromethamine RS from the Standard stock solution and 0.03 mg/mL of Internal standard solution in Diluent

Sample stock solution:  Nominally 0.24 mg/mL of ketorolac tromethamine in methanol, from an equivalent volume of Injection.

Sample solution:  Transfer 5.0 mL of the Sample stock solution and 5.0 mL of the Internal standard solution to a 50-mL volumetric flask, and dilute with Diluent to volume.

Chromatographic system 

(See Chromatography 621 , System Suitability.)

Mode:  LC

Detector:  UV 254 nm

Column:  4.6-mm × 25-cm; 5-µm packing L1

Flow rate:  1.2 mL/min

Injection volume:  100 µL

System suitability 

Sample:  Standard solution

[NOTE— The relative retention times for ketorolac and naproxen are 0.7 and 1.0, respectively. ]

Resolution:  NLT 5.4 between ketorolac and naproxen

Column efficiency:  NLT 2700 theoretical plates for the ketorolac peak

Tailing factor:  NMT 1.5 for the ketorolac peak

Relative standard deviation:  NMT 1.5%

Analysis 

Samples:  Standard solution and Sample solution

Calculate the percentage of ketorolac tromethamine (C15H13NO3 · C4H11NO3 ) in each mL of Injection taken:

Result = ( R U / R S ) × ( C S / C U ) × 100

 

R U	=	= peak response ratio of ketorolac to naproxen from the Sample solution
R S	=	= peak response ratio of ketorolac to naproxen from the Standard solution
C S	=	= concentration of USP KetorolacTromethamine RS in the Standard solution (mg/mL)
C U	=	= nominal concentration of ketorolactromethamine in the Sample solution(mg/mL)

Acceptance criteria:  90.0%–110.0%

SPECIFIC TESTS

•   pH 791 : 6.9–7.9

•   Bacterial Endotoxins Test 85 : It contains NMT 5.8 USP Endotoxin Units/mg of ketorolac tromethamine.

•   Sterility Tests 71 : Meets the requirements for Test for Sterility of the Product to Be Examined, Membrane Filtration

•   Particulate Matter in Injections 788 : Meets the requirements for small-volume injections

•  Other Requirements: Meets the requirements for Injections 1

ADDITIONAL REQUIREMENTS

•  Packaging and Storage: Preserve in single-dose containers, preferably of Type I glass, protected from light, and store at controlled room temperature.

•   USP Reference Standards 11

USP Endotoxin RS

USP Ketorolac Tromethamine RS 

Auxiliary Information— Please check for your question in the FAQs before contacting USP.

 

 

 

Topic/Question	Contact	Expert Committee
Monograph	Hillary Z Cai  Scientific Liaison, Small Molecules (301) 230-3379	(SM22010) Monographs - Small Molecules 2
85	Radhakrishna S Tirumalai, Ph.D.  Principal Scientific Liaison (301) 816-8339	(GCM2010) General Chapters - Microbiology
71	Radhakrishna S Tirumalai, Ph.D.  Principal Scientific Liaison (301) 816-8339	(GCM2010) General Chapters - Microbiology
Reference Standards	RS Technical Services 1-301-816-8129 rstech@usp.org

USP38–NF33 Page 4011

Pharmacopeial Forum: Volume No. 40(4)