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Ticarcillin Monosodium
C15H15N2NaO6S2·H2O 424.43

4-Thia-1-azabicyclo[3.2.0]heptane-2-carboxylic acid, 6-[(carboxy-3-thienylacetyl)amino]-3,3-dimethyl-7-oxo, monosodium salt, [2S-2,5,6(S*)]-, monohydrate.

(R)-N-[(2S,5R,6R)-2-Carboxy-3,4-dimethyl-7-oxo-4-thia-1-azabicyclo[3.2.0]hept-6-yl-]3-thiophenemalonamic acid monosodium salt.

Anhydrous 406.42 [74682-62-5].
» Ticarcillin Monosodium contains the equivalent of not less than 890 µg of ticarcillin (C15H16N2O6S2) per mg, calculated on the anhydrous basis.
Packaging and storage— Preserve in tight containers.
Labeling— Where it is intended for use in preparing injectable dosage forms, the label states that it is sterile or must be subjected to further processing during the preparation of injectable dosage forms.
Identification—
B: Ultraviolet Absorption 197U—
Solution: 20 µg per mL, obtained as follows. Transfer about 40 mg, accurately weighed, to a 100-mL volumetric flask, dissolve in and dilute with water to volume, and mix. Transfer 5.0 mL of this solution to a second 100-mL volumetric flask, dilute with 0.1 N methanolic hydrochloric acid (0.8 mL of hydrochloric acid diluted with methanol to 100 mL) to volume, and mix. Record the spectrum between 200 and 300 nm.
C: A solution (1 in 20) responds to the tests for Sodium 191.
Specific rotation 781S: between +181 and +197.
Test solution: 10 mg per mL, in pH 6.4 sodium phosphate buffer, prepared as directed in the Assay.
Crystallinity 695: meets the requirements.
pH 791: between 2.5 and 4.0, in a solution containing the equivalent of 10 mg of ticarcillin per mL.
Water, Method I 921: between 4.0% and 6.0%.
Dimethylaniline 223: meets the requirement.
Residual solvents 467: meets the requirements.
(Official January 1, 2007)
Other requirements— Where the label states that Ticarcillin Monosodium is sterile, it meets the requirements for Sterility 71 and for Bacterial endotoxins under Ticarcillin for Injection. Where the label states that Ticarcillin Monosodium must be subjected to further processing during the preparation of injectable dosage forms, it meets the requirements for Bacterial endotoxins under Ticarcillin for Injection.
Assay—
pH 4.3 sodium phosphate buffer— Dissolve 13.8 g of monobasic sodium phosphate in 900 mL of water, adjust with phosphoric acid or 10 N sodium hydroxide to a pH of 4.3 ± 0.1, dilute with water to make 1000 mL, and mix.
Mobile phase— Prepare a suitable mixture of pH 4.3 sodium phosphate buffer and acetonitrile (95:5), and pass through a membrane filter of 0.5-µm or finer porosity. Make adjustments if necessary (see System Suitability under Chromatography 621).
pH 6.4 sodium phosphate buffer— Dissolve 6.9 g of monobasic sodium phosphate in 900 mL of water, adjust with 10 N sodium hydroxide to a pH of 6.4 ± 0.1, dilute with water to make 1000 mL, and mix.
Standard preparation— Transfer about 50 mg of USP Ticarcillin Monosodium Monohydrate RS, accurately weighed, to a 50-mL volumetric flask, dilute with pH 6.4 sodium phosphate buffer to volume, and mix.
Resolution solution— Transfer about 25 mg of USP Ticarcillin Monosodium Monohydrate RS, accurately weighed, to a 25-mL volumetric flask. Prepare a solution of USP Clavulanate Lithium RS in pH 6.4 sodium phosphate buffer containing the equivalent of about 0.15 mg of clavulanic acid per mL. Place 5 mL of this solution in the 25-mL volumetric flask, dilute with pH 6.4 sodium phosphate buffer to volume, and mix. [NOTE—Use this solution on the day prepared.]
Assay preparation— Transfer about 50 mg of Ticarcillin Monosodium, accurately weighed, to a 50-mL volumetric flask, dilute with pH 6.4 sodium phosphate buffer to volume, and mix.
Chromatographic system (see Chromatography 621)—The liquid chromatograph is equipped with a 220-nm detector and a 4-mm × 30-cm column that contains 3- to 10-µm packing L1. The flow rate is about 2 mL per minute. Chromatograph the Resolution solution, and record the peak responses as directed for Procedure: the relative retention times are about 0.2 for clavulanic acid and 1.0 for ticarcillin; and the resolution, R, between the clavulanic acid peak and the ticarcillin peak is not less than 5.0. Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the column efficiency is not less than 1000 theoretical plates; the tailing factor is not more than 2.0; 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 preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the responses for the major peaks. Calculate the quantity, in µg, of ticarcillin (C15H16N2O6S2) in each mg of the Ticarcillin Monosodium taken by the formula:
50(CP / W)(rU / rS),
in which C is the concentration, in mg per mL, of USP Ticarcillin Monosodium Monohydrate RS in the Standard preparation; P is the designated potency, in µg of ticarcillin (C15H16N2O6S2) per mg, of USP Ticarcillin Monosodium Monohydrate RS; W is the weight, in mg, of Ticarcillin Monosodium taken to prepare the Assay preparation; and rU and rS are the ticarcillin peak responses obtained from the Assay preparation and the Standard preparation, respectively.
Auxiliary Information— Staff Liaison : Brian D. Gilbert, Ph.D., Scientist
Expert Committee : (MDANT05) Monograph Development-Antibiotics
USP29–NF24 Page 2147
Phone Number : 1-301-816-8223