Printed on: Mon Aug 02 2021, 06:41:39 PM Official Status: Currently Official on 02-Aug-2021 DocId: 1_GUID-440BDE2C-E368-47A5-A4B9-F283CA8AF77B_4_en-US

(EST)
Printed by: Le Tran Official Date: Official as of 01-May-2020 Document Type: USP @2021 USPC
1

Mode: LC
Ticarcillin Disodium Detector: UV 220 nm
Column: 4-mm × 25-cm; 5-µm packing L1
Flow rate: 1 mL/min
Injection volume: 20 µL
System suitability
Sample: Standard solution
Suitability requirements
Resolution: NLT 1.5 between the two ticarcillin peaks
Relative standard deviation: NMT 1.0% for the sum of
the ticarcillin peaks
Analysis
Samples: Standard solution and Sample solution
Calculate the quantity, in µg/mg, of ticarcillin
(C15H16N2O6S2) in the portion of Ticarcillin Disodium
taken:

C15H14N2Na2O6S2 428.38 Result = (r U/r S) × (C S/C U) × P

4-Thia-1-azabicyclo[3.2.0]heptane-2-carboxylic acid, 6- rU = sum of the responses of the two ticarcillin peaks
[(carboxy-3-thienylacetyl)amino]-3,3-dimethyl-7-oxo-, from the Sample solution
disodium salt, [2S-[2α,5α,6β(S*)]]-; rS = sum of the responses of the two ticarcillin peaks
N-(2-Carboxy-3,3-dimethyl-7-oxo-4-thia-1-azabicyclo[3.2.0] from the Standard solution

al
hept-6-yl)-3-thiophenemalonamic acid disodium salt CS = concentration of USP Ticarcillin Monosodium
[4697-14-7]. Monohydrate RS in the Standard solution
DEFINITION (mg/mL)
Ticarcillin Disodium has a potency equivalent to NLT 800 µg/ CU = concentration of Ticarcillin Disodium in the
mg of ticarcillin (C15H16N2O6S2), calculated on the anhydrous Sample solution (mg/mL)
basis.
IDENTIFICATION
ci P = potency of ticarcillin in USP Ticarcillin
Monosodium Monohydrate RS (µg/mg)

Acceptance criteria: NLT 800 µg/mg on the anhydrous

Change to read: basis
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• A. ▲SPECTROSCOPIC IDENTIFICATION TESTS á197ñ, Infrared IMPURITIES
Spectroscopy: 197K▲ (CN 1-May-2020) • DIMETHYLANILINE á223ñ: Meets the requirements
Solution A: Acetone and water (90:10) • ORGANIC IMPURITIES
Standard: Dissolve 50 mg of USP Ticarcillin Monosodium Solution A: 1.3 g/L of dibasic ammonium phosphate in
Monohydrate RS in 1 mL of water, add 0.1 mL of water adjusted with phosphoric acid to a pH of 7.0
hydrochloric acid, swirl, and allow to stand in iced water for Solution B: Methanol and Solution A (50:50)
O

10 min. Pass through a filter. Wash the residue with 2 mL Mobile phase: See Table 1.
of water and dissolve in Solution A. Evaporate almost to
dryness, then dry in an oven at 60° for 30 min. Table 1
Sample: Dissolve 50 mg of Ticarcillin Disodium in 1 mL of Time Solution A Solution B
water, add 0.1 mL of hydrochloric acid, swirl, and allow to (min) (%) (%)
stand in iced water for 10 min. Pass through a filter. Wash
the residue with 2 mL of water and dissolve in Solution A. 0 100 0
Evaporate almost to dryness, then dry in an oven at 60° for 30 30 70
30 min.
Acceptance criteria: Meets the requirements 40 30 70
• B. Meets the requirements of the test for Optical Rotation,
Specific Rotation System suitability solution: 0.02 mg/mL of USP Ticarcillin
• C. The retention times of the major peaks of the Sample Monosodium Monohydrate RS in Solution A
solution correspond to those of the Standard solution, as Sample solution: 1 mg/mL of Ticarcillin Disodium in
obtained in the Assay. Solution A
• D. IDENTIFICATION TESTS—GENERAL, Sodium á191ñ Chromatographic system
Sample solution: 50 mg/mL (See Chromatography á621ñ, System Suitability.)
Acceptance criteria: Meets the requirements Mode: LC
Detector: UV 220 nm
ASSAY Column: 4-mm × 25-cm; 5-µm packing L1
• PROCEDURE Flow rate: 1 mL/min
Buffer: 1.3 g/L of dibasic ammonium phosphate in water Injection volume: 20 µL
adjusted with phosphoric acid to a pH of 7.0 System suitability
Mobile phase: Methanol and Buffer (20:80) Sample: System suitability solution
Standard solution: 0.1 mg/mL of USP Ticarcillin Suitability requirements
Monosodium Monohydrate RS in Mobile phase Resolution: NLT 2.0 between the two ticarcillin peaks
Sample solution: 0.1 mg/mL of Ticarcillin Disodium in Relative standard deviation: NMT 5.0% for the sum of
Mobile phase the ticarcillin peaks
Chromatographic system Analysis
(See Chromatography á621ñ, System Suitability.) Sample: Sample solution

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Printed on: Mon Aug 02 2021, 06:41:39 PM Official Status: Currently Official on 02-Aug-2021 DocId: 1_GUID-440BDE2C-E368-47A5-A4B9-F283CA8AF77B_4_en-US
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Printed by: Le Tran Official Date: Official as of 01-May-2020 Document Type: USP @2021 USPC
2

Calculate the percentage of each impurity in the portion of Acceptance criteria: +172° to +187°
Ticarcillin Disodium taken: • PH á791ñ
Sample solution: 10 mg/mL of ticarcillin from Ticarcillin
Result = (r U/r T) × 100 Disodium in water
Acceptance criteria: 6.0–8.0
rU = peak response of each impurity from the Sample • WATER DETERMINATION, Method I á921ñ: NMT 6.0%
solution • STERILITY TESTS á71ñ: Where the label states that Ticarcillin
rT = sum of the responses of the two ticarcillin peaks Disodium is sterile, it meets the requirements in Test for
from the Sample solution Sterility of the Product to Be Examined, Membrane Filtration.
• BACTERIAL ENDOTOXINS TEST á85ñ: Where the label states
Acceptance criteria: See Table 2. that Ticarcillin Disodium is sterile or must be subjected to
further processing during the preparation of injectable
Table 2 dosage forms, it contains NMT 0.05 USP Endotoxin
Relative Acceptance Units/mg of ticarcillin.
Retention Criteria,
Name Time NMT (%) ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in tight containers and
0.95
— store in a refrigerator.
Ticarcillin 1.0 • LABELING: Where it is intended for use in preparing
Ticarcillin related com-
injectable dosage forms, the label states that it is sterile or
pound Aa 2.1 4 must be subjected to further processing during the
preparation of injectable dosage forms.
Any individual • USP REFERENCE STANDARDS á11ñ

al
unspecified —
impurity 2.5 USP Ticarcillin Monosodium Monohydrate RS
C15H15N2NaO6S2 · H2O 424.42
a Decarboxy ticarcillin; (2S,5R,6R)-3,3-Dimethyl-7-oxo-6-[[(thiophen-3-yl)
acetyl]amino]-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxylic acid.

SPECIFIC TESTS
• OPTICAL ROTATION, Specific Rotation á781Sñ
Sample solution: 10 mg/mL in water
ci
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