Raw Material Specification & Method of Analysis (MOA) / Standard Testing Procedure (STP) for Succinic Acid USP and per USP NF Volume No. PF 41(4).

Specification of Succinic Acid USP

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Analytical Method of Succinic Acid USP

1.0     Description

• • Carry out the test on sample as per procedure. For detailed Description Test Procedure – Refer GTP – Description / Appearance Test.

2.0     Solubility

• • Freely soluble in boiling water; soluble in water, in alcohol, and in glycerin. 

• • Carry out the test as per procedure of solubility check.

Solubility Table

3.0     Identification

• • Test A (By IR)

• • The Infrared absorption spectrum should be concordant with reference spectrum of that standard.  Carry out the test as per procedure.

• • Test B

• • The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.

4.0     Melting Range or Temperature

• • Carry out the test as per respective handling procedure of Melting Point Apparatus.

5.0     Residue on Ignition of  Succinic Acid USP

• Carry out the test as per below procedure.

• • Prepare Crucible: Ignite a clean, dry silica or platinum crucible at 600 ± 50°C for 30 minutes, cool in a desiccator, and weigh accurately (W1).

• • Weigh Sample: Accurately weigh 1-2g (or as specified) of the substance into the crucible.

• • Charring: Moisten the sample with about 1 mL of sulfuric acid and heat gently at the lowest practicable temperature until thoroughly charred (blackened).

• • Further Heating: Cool, then carefully add another 1 mL of sulfuric acid to the residue.

• • Heat gently until white fumes are no longer evolved.

• • Ignition: Ignite in a muffle furnace at 600 ± 50°C (or specified temp) until all black particles disappear and the residue is completely incinerated (usually 2 hours).

• • Ensure no flames appear.

• • Cool & Weigh: Cool the crucible in a desiccator and weigh accurately (W2).

• • Constant Weight: Repeat the ignition, cooling, and weighing steps until two successive weighings (W2 and W3) do not differ by more than 0.5 mg.

• •  Calculate Percentage: (Weight of final residue (W2-W1) / Weight of original sample) * 100.

6.0     Assay of Succinic Acid USP

• Procedure :

• • Diluent : Dissolve 6.8 g of potassium phosphate monobasic in 2 L of water. Adjust the pH of the solution to 2.3 with drops of phosphoric acid. This solution is 25 M potassium phosphate buffer, pH 2.3.

• • Mobile phase : Methanol and Diluent (8:92)

• • System suitability solution : 1.0 mg/mL of USP Succinic Acid RS and 0.003 mg/mL of USP Fumaric Acid RS in Diluent

• • Standard solution : 1.0 mg/mL of USP Succinic Acid RS in Diluent

( Dilution : 50mg———-> 50ml )

• • Sample solution : 1.0 mg/mL of Succinic Acid in Diluent

( Dilution : 50mg———> 50ml )

• • Chromatographic system

• • • Mode : LC

• • • Detector : UV 204 nm

• • • Column : 4.6-mm × 15-cm; 3-µm packing L1

• • • Flow rate : 1.0 mL/min

• • • Injection volume : 20 µL

• • System suitability

• • Sample : System suitability solution

[Note— The relative retention times for succinic acid and fumaric acid are 1.0 and 1.2, respectively. ]

• •  Suitability requirements

• • Resolution : NLT 2.0 between succinic acid and fumaric acid

• • Relative standard deviation: NMT 0.5% for the succinic acid peak

• • Tailing factor : 0.8–2.0

• • Analysis

• • Samples : Standard solution and Sample solution

• • Calculate the percentage of succinic acid (C4H6O4 ) in the portion of succinic acid taken:

• • Result = ( r U / r S ) × ( C S / C U ) × 100

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