(tye' loe sin tar' trate).
Tylosin A (Tylosin) 916.10 [1401-69-0].
» Tylosin Tartrate is a tartrate of a mixture of macrolide antibiotic substances, or the mixture of such substances, produced by the growth of Streptomyces fradiae, or by any other means. Its potency is not less than 800 µg of tylosin per mg, calculated on the dried basis.
Packaging and storage Preserve in well-closed containers, protected from light, moisture, and excessive heat. Store at 25, excursions permitted between 15 and 30.
Labeling Label it to indicate that it is for veterinary use only.
USP Reference standards 11
USP Tylosin Tartrate RS
A: Infrared Absorption 197K.
B: The retention time of the major peak for tylosin A in the chromatogram of the Test solution corresponds to that in the chromatogram of the Standard solution, as obtained in the test for Content of tylosins.
C: It meets the requirements of the test for Tartrate 191.
pH 791: between 5.0 and 7.2 in a solution prepared by dissolving 0.25 g in 10 mL of carbon dioxide-free water.
Loss on drying 731 Dry about 1 g, accurately weighed, in vacuum at a pressure not exceeding 5 mm of mercury at 60 for 3 hours: it loses not more than 4.5% of its weight.
Residue on ignition 281: not more than 2.5%, the charred residue being moistened with 2 mL of nitric acid and 5 drops of sulfuric acid.
Limit of tyramine In a 25-mL volumetric flask, dissolve 50.0 mg of tylosin in 5.0 mL of a 3.4 g per L solution of phosphoric acid. Add 1.0 mL of pyridine and 2.0 mL of a saturated solution of ninhydrin (about 40 g per L). Close the flask with aluminum foil, and heat in a water bath at 85 for 30 minutes. Cool the solution rapidly to room temperature, and dilute with water to volume. Mix, and measure immediately the absorbance (see Spectrophotometry and Light-Scattering 851) of the solution at 570 nm against a blank solution prepared in a similar manner. The absorbance is not greater than that of a standard prepared at the same time and in the same manner using 5.0 mL of a 35 mg per L solution of tyramine in a 3.4 g per L solution of phosphoric acid. If intended for use in the manufacture of parenteral dosage forms, the absorbance is not greater than that of a standard prepared at the same time and in the same manner using 5.0 mL of a 15 mg per L solution of tyramine in a 3.4 g per L solution of phosphoric acid.
Content of tylosins
Mobile phase Prepare a mixture of filtered 200 g per L of sodium perchlorate, previously adjusted with 1 N hydrochloric acid to a pH of 2.5 ± 0.1, and acetonitrile (60:40). Make adjustments if necessary (see System Suitability under Chromatography 621).
Standard solution Dissolve an accurately weighed quantity of USP Tylosin RS in a mixture of acetonitrile and water (1:1) to obtain a solution having a known concentration of about 0.2 mg per mL. [notePrepare the Standard solution immediately before use. ]
Test solution Dissolve an accurately weighed quantity of Tylosin in a mixture of acetonitrile and water (1:1) to obtain a solution having a known concentration of about 0.2 mg per mL. [notePrepare the Test solution immediately before use. ]
Chromatographic system (see Chromatography 621) The liquid chromatograph is equipped with a 290-nm detector and a 4.6-mm × 20-cm column that contains 5-µm packing L1. The flow rate is about 1.0 mL per minute and the column temperature is maintained at 35. Chromatograph the Standard solution, and record the peak responses as directed for Procedure: the order of elution is tylosin C, tylosin B, tylosin D, and tylosin A with relative retention times of about 0.5, 0.6, 0.8, and 1.0 minutes, respectively; the resolution of the peaks representing tylosin D and tylosin A is not less than 2.0; the tailing factors are not more than 1.5; and the relative standard deviation for replicate injections is not more than 2.0%.
Procedure Separately inject equal volumes (about 20 µL) of the Standard solution and the Test solution into the chromatograph, record the chromatograms over a period of time equivalent to 1.5 times the elution time of the main tylosin A peak, and measure the peak areas for all the peaks. Calculate the percentages of tylosin A, tylosin B, tylosin C, and tylosin D in the Tylosin taken by the formula:
100(rI / rs)in which rI is the area of the tylosin A peak, the tylosin B peak, the tylosin C peak, or the tylosin D peak, as appropriate, in the chromatogram obtained from the Test solution; and rs is the sum of the areas of all the peaks in the chromatogram obtained from the Test solution: the content of tylosin A is not less than 80%; and the sum of the contents of tylosin A, tylosin B, tylosin C, and tylosin D is not less than 95%.
Assay Proceed as directed for Tylosin under AntibioticsMicrobial Assays 81. Prepare the Test Dilution as follows. Transfer an accurately weighed quantity of Tylosin Tartrate, equivalent to about 250 mg of tylosin, to a 500-mL volumetric flask, add 50 mL of methanol, and swirl to dissolve. Dilute with Buffer No. 3 to volume, and mix. Transfer 4.0 mL of this solution to a second 500-mL volumetric flask, dilute with a mixture of Buffer No. 3 and methanol (1:1), and mix. This solution contains about 4 µg of tylosin per mL.
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