Methylergonovine Maleate Injection
DEFINITION
Methylergonovine Maleate Injection is a sterile solution of Methylergonovine Maleate in Water for Injection. Each mL contains NLT 90.0% and NMT 110.0% of the labeled amount of methylergonovine maleate (C20H25N3O2·C4H4O4).
IDENTIFICATION
• A.
The RF values of the principal fluorescent spot and the principal blue spot of the Sample solution correspond to those of the Standard stock solution, as obtained in the procedure for Organic Impurities, Related Alkaloids.
• B. Procedure
Sample solution:
0.67 mg/mL of methylergonovine maleate from Injection in water
Analysis:
The Sample solution exhibits a bluish fluorescence under UV light. To this solution add 2 mL of a solution of glacial acetic acid in ethyl acetate (1:2), and stratify 2 mL of sulfuric acid, by pipetting, under the solution.
Acceptance criteria:
A bluish-purple ring appears at the interface of the two liquids.
ASSAY
• Procedure
[Note—Conduct this procedure with minimum exposure to light. ]
Mobile phase:
Acetonitrile and 0.015 M monobasic potassium phosphate solution (1:4)
Diluent:
5 mg/mL of tartaric acid in water and methanol (1:1). Allow the mixture to cool before use. [Note—Dissolve tartaric acid with water, then add an equal volume of methanol. ]
Standard solution:
100 µg/mL of USP Methylergonovine Maleate RS in Diluent. [Note—Shake by mechanical means for 15 min or until completely dissolved. ]
Sample solution:
100 µg/mL of methylergonovine maleate from Injection in Diluent
Chromatographic system
Mode:
LC
Detector:
UV 240 nm
Column:
4-mm × 25-cm; packing L7
Column temperature:
30
Flow rate:
2 mL/min
Injection size:
20 µL
System suitability
Sample:
Standard solution
Suitability requirements
Column efficiency:
NLT 1000 theoretical plates
Tailing factor:
NMT 2.0
Relative standard deviation:
NMT 2.0%
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of C20H25N3O2·C4H4O4 in each mL of Injection taken:
Result = (rU/rS) × (CS/CU) × 100
| rU | = | = peak response from the Sample solution |
| rS | = | = peak response from the Standard solution |
| CS | = | = concentration of USP Methylergonovine Maleate RS in the Standard solution (µg/mL) |
| CU | = | = nominal concentration of the Sample solution (µg/mL) |
Acceptance criteria:
90.0%–110.0%
IMPURITIES
Organic Impurities
• Procedure: Related Alkaloids
[Note—Conduct this test promptly, without exposure to daylight and with minimum exposure to artificial light. ]
Diluent:
Alcohol and ammonium hydroxide (9:1)
[Note—All solutions should be prepared immediately before use. ]
Standard stock solution:
10 mg/mL of USP Methylergonovine Maleate RS in Diluent
Standard solution A:
0.50 mg/mL of USP Methylergonovine Maleate RS from the Standard stock solution in Diluent
Standard solution B:
0.20 mg/mL of USP Methylergonovine Maleate RS from the Standard stock solution in Diluent
Standard solution C:
0.10 mg/mL of USP Methylergonovine Maleate RS from the Standard stock solution in Diluent
Standard solution D:
0.05 mg/mL of USP Methylergonovine Maleate RS from the Standard stock solution in Diluent
Sample solution:
Transfer the equivalent of 5 mg of methylergonovine maleate from Injection to a separator, and extract with three 5-mL portions of chloroform. Discard the chloroform extracts. Render alkaline to litmus with 6 N ammonium hydroxide, and extract with three 5-mL portions of chloroform. Evaporate the combined extracts with the aid of a current of air, but without heat, to dryness. Dissolve the residue so obtained in 0.5 mL of Diluent.
Chromatographic system
Mode:
TLC
Adsorbent:
0.25-mm layer of chromatographic silica gel mixture
Application volume:
5 µL
Developing solvent system:
Chloroform, methanol, and water (75:25:3), equilibrated for 30 min
Spray reagent:
10 mg/mL of p-dimethylaminobenzaldehyde in a cooled mixture of alcohol and hydrochloric acid (1:1)
Analysis
Samples:
Standard stock solution, Standard solution A, Standard solution B, Standard solution C, Standard solution D, and Sample solution
Proceed as directed in the chapter. Locate the spots on the plate by spraying thoroughly and evenly with Spray reagent. Immediately dry in a stream of nitrogen for 2 min.
Acceptance criteria:
The RF value of the principal spot from the Sample solution corresponds to that from the Standard stock solution. Estimate the concentration of any other spots observed in the lane for the Sample solution by comparison with Standard solution A, Standard solution B, Standard solution C, and Standard solution D: the spots from the 0.50-, 0.20-, 0.10-, and 0.05-mg/mL dilutions are equivalent to 5.0%, 2.0%, 1.0%, and 0.50% of impurities, respectively. The sum of the impurities is NMT 5.0%.
SPECIFIC TESTS
• pH 
791
:
2.7–3.5
791:
2.7–3.5
• Bacterial Endotoxins Test 85:
NMT 1.7 USP Endotoxin Units/µg of methylergonovine maleate
85:
NMT 1.7 USP Endotoxin Units/µg of methylergonovine maleate
• Other Requirements:
Meets the requirements under Injections 1
1
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in single-dose, light-resistant containers, preferably of Type I glass. Store in a refrigerator.
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Auxiliary Information—
Please check for your question in the FAQs before contacting USP.
| Topic/Question | Contact | Expert Committee |
|---|---|---|
| Monograph | Mary S. Waddell
Scientific Liaison 1-301-816-8124 |
(SM42010) Monographs - Small Molecules 4 |
| 85 |
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 3878
Pharmacopeial Forum: Volume No. 36(4) Page 929