Calcitonin Salmon Nasal Solution
DEFINITION
Calcitonin Salmon Nasal Solution is a solution of Calcitonin Salmon in a suitable diluent. It contains suitable preservatives, and is packaged in a form suitable for nasal administration so that the required dosage can be controlled as required. Each mL of Calcitonin Salmon Nasal Solution possesses an activity of NLT 80% and NMT 115% of that stated on the label.
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
Solution A:
3.26 mg/mL of tetramethylammonium hydroxide pentahydrate in water and acetonitrile (9:1). Adjust with phosphoric acid to a pH of 2.5.
Solution B:
1.45 mg/mL of tetramethylammonium hydroxide pentahydrate in acetonitrile and water (3:2). Adjust with phosphoric acid to a pH of 2.5.
Mobile phase:
See the gradient table below.
| Time (min) |
Solution A (%) |
Solution B (%) |
|---|---|---|
| 0 | 72 | 28 |
| 30 | 48 | 52 |
| 32 | 72 | 28 |
| 55 | 72 | 28 |
Diluent:
7.5 mg/mL of sodium chloride, 2 mg/mL of sodium acetate, and 2 mg/mL of glacial acetic acid in water
Standard stock solution:
1.0 mg/mL of USP Calcitonin Salmon RS in Solution A
Standard solution:
0.1 mg/mL of USP Calcitonin Salmon RS from the Standard stock solution in Solution A
System suitability stock solution:
Dissolve the contents of a vial of USP Calcitonin Salmon Related Compound A RS in 0.4 mL of Solution A, and add 0.1 mL of the Standard solution.
System suitability solution:
System suitability stock solution and Solution A (1:9)
Sample solution:
Nasal Solution in Diluent (1:9)
Chromatographic system
Mode:
LC
Detector:
UV 220 nm
Column:
4.6-mm × 25-cm; packing L1
Column temperature:
65
Flow rate:
1 mL/min
Injection size:
200 µL
System suitability
Samples:
Standard solution and System suitability solution
[Note—The relative retention times for calcitonin salmon and calcitonin salmon related compound A are 1.0 and 1.15, respectively. ]
Suitability requirements
Resolution:
NLT 3 between calcitonin salmon and calcitonin salmon related compound A
Tailing factor:
NMT 2.5
Relative standard deviation:
NMT 3.0%
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of Calcitonin Salmon in the portion of Nasal Solution taken:
Result = (rU/rS) × (CS/CU) × 100
| rU | = | = peak area of the Sample solution |
| rS | = | = peak area of the Standard solution |
| CS | = | = concentration of USP Calcitonin Salmon RS in the Standard solution (mg/mL) |
| CU | = | = nominal concentration of calcitonin salmon in the Sample solution (mg/mL) |
Acceptance criteria:
80%–115%
SPECIFIC TESTS
• Microbial Enumeration Tests 
61
and Tests for Specified Microorganisms 62:
The total aerobic microbial count is NMT 100 cfu/g, and the total combined molds and yeasts count is NMT 50 cfu/g. It meets the requirements for absence of Staphylococcus aureus and Pseudomonas aeruginosa.
61 and Tests for Specified Microorganisms 62:
The total aerobic microbial count is NMT 100 cfu/g, and the total combined molds and yeasts count is NMT 50 cfu/g. It meets the requirements for absence of Staphylococcus aureus and Pseudomonas aeruginosa.
• pH 791:
3.5–4.5
791:
3.5–4.5
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in containers suitable for spraying the contents into the nasal cavities in a controlled individualized dosage. Store unopened containers in a refrigerator and opened containers at room temperature.
• Labeling:
Label it to indicate that it is for intranasal administration only. The labeling also states that it has been prepared either with Calcitonin Salmon of synthetic origin or Calcitonin Salmon of rDNA origin. Label it to state that it is to be stored in a refrigerator, and that freezing is to be avoided. Label it to indicate the activity in USP Calcitonin Salmon Units per mL.
• USP Reference Standards 11
11
USP Calcitonin Salmon RS
USP Calcitonin Salmon Related Compound A RS 
N-Acetyl-cys1-calcitonin.
C146H243N44O49S2 3463
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N-Acetyl-cys1-calcitonin.
C146H243N44O49S2 3463
Auxiliary Information—
Please check for your question in the FAQs before contacting USP.
| Topic/Question | Contact | Expert Committee |
|---|---|---|
| Monograph | Thomas A. Sigambris, M.S.
Scientific Liaison 1-301-998-6789 |
(BIO12010) Monographs - Biologics and Biotechnology 1 |
| 61 |
Radhakrishna S Tirumalai, Ph.D.
Principal Scientific Liaison 1-301-816-8339 |
(GCM2010) General Chapters - Microbiology |
| 62 |
Radhakrishna S Tirumalai, Ph.D.
Principal Scientific Liaison 1-301-816-8339 |
(GCM2010) General Chapters - Microbiology |
| Reference Standards | RS Technical Services 1-301-816-8129 rstech@usp.org |
USP35–NF30 Page 2437
Pharmacopeial Forum: Volume No. 32(3) Page 767