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1 Hon [100%]121 e-mail: teruyuki_kitagawa ZASSHI122(1) 121 125 (2002) 2002 The Pharmaceutical Society of Japan Notes Studies on Residue on Ignition Test in JPTeruyuki KITAGAWA,YumiUMEYAMA,KaoruHIRATA, and Shigetaka KODA Fujisawa Pharmaceutical Co., Ltd., Analytical Research Laboratories, 2 1 6,Kashima, Yodogawa-ku, Osaka 532 8514, Japan(Received August 17, 2001; Accepted October 31, 2001)The Residue on Ignition Test speci ed in General Tests, Japanese Pharmacopeia is a method to measure the weightof the residual substance not volatilized when the sample is ignited under a constant condition. Generally, this test is in-tended to determine the content of inorganic substances contained as impurities in an organic substance, and, oc-casionally, to determine the amount of inorganic substances contained as components in an organic substance. Ourlaboratories have adopted this test method for the above two purposes in the case of the quality control for drug sub-stances, synthetic intermediates, starting materials in the course of drug development.

2 Some validation studies have beenconducted for this test in order to clarify the quantitation limit in the case of an application for the former purpose, andtrueness and precision in the case of the latter purpose. Consequently, the quantitation limit was determined as mg. The amount of sample should be determined based on this quantitation limit(mg)and the level of quantitationlimit( )or that of speci cation limit( )should be considered from the view point of each testing purpose. The testmethod was also con rmed to have a good trueness and precision as the determination method for an alkaline salt, suchas sodium, potassium or calcium salt, of organic compounds, as long as the test is operated with great care not to scatterthe content out of crucible during ignition to words residue on ignition; validation; quantitation limit; trueness; precision 14 14 JP14 1) 1.

3 13 12 hon [100%]122 Table 1. Results of Residue on Ignition Test for Various Kinds of Inorganic CompoundsInorganic compoundNaCl NaNO3Na2 HPO4 NaBF4 KBrKBrO3NH4Cl(NH4)2SO4 Expected weighing formNa2SO4Na2SO4Na2SO4Na2SO4K2SO4K2SO4 Theoretical residue on ignition( )[A] residue on ignition( )[B] [B] [A] It needed a very long time to get a constant weight of residue on ignition. The thoretical residue on ignition was when corrected with the amountof NaF contained in 122 (2002)JIS C23H14Na2O11 C17H11N6 NaO3 H2O C6H11KO7 C6H4(COOK)(COOH C12H14 CaO12 2H2O C12H22 CaO14 6 2.)

4 1712MP8 2024MP6 R200D MFP 300N FP 41 3. 14 550 C 1. 8 100 mg Table 1 6 2 X PtP2 2) 3) 2. mg/mL , , , 1mL mg, mg, , mg mg hon [100%]123 Table 2.

5 Repeatability of Amount(mg)of the Residue Ob-tained by Residue on Ignition Test with Di erent Amount ofSodium Sulfate(Na2SO4)Added amount ofsodium sulfate(mg) ( ) (Note)Each value in the table represents amount(mg)of residueweighed after ignition to constant 3. Intermediate Precision of Amount(mg)of theResidue Obtained by Residue on Ignition Test with Di erentAmount of Sodium Sulfate(Na2SO4)Added amountof sodiumsulfate(mg)Testingdate12345 Replicatenumbern 6n 6n 6n 6n ( ) ( ) (Note)Each value in the table represents amount(mg)of residueweighed after ignition to constant 1. Relationship between added amount of sodium sul-fate and repeatability of residue on ignition123No.

6 1 6 mg mg Table 2 Fig. 1 mg mg mg mg mg Table 3 mg mg 10 10 mg mg d 95 d s 95 0 mg mg g 1g hon [100%]124 Table 4. Results of Metal Content in Sodium, Potassium and Calcium Salt Compounds Determined by Residue on Ignition TestSample compoundReplicatenumberResidue on ignition( )([A] [B]) 100(Range, Mean, )Theoretical value[A]Determined value[B](Range)Sodium , , , , C17H11N6 NaO3 , , , , Potassium , , , , , , C6H4(COOK)(COOH) , , Calcium saltCaCl2 , , Ca(NO3)2 , , C12H14 CaO12 , , , , These values were calculated as anhydrous 5.

7 Relationship between Ignition Method and Metal Content of Calcium GluconateIgnition methodReplicatenumberResidue on ignition( )([A] [B]) 100(Range, Mean, )Theoretical value[A]Determined value[B](Range)With Bunsen , , Without Bunsen burner , , Sand bath was employed instead of Bunsen burner and controlled at about 300 122 (2002)3. 2 4 g ) [ ( )/ ( ) 100 ( ) Table 4 3 99 1 3 300 C 550 C Table 5 hon [100%]125125No.]

8 1 mg PDG USP, EP JP 2000 11 600 50 C 4) 14 1 14 450 550 C 550 C 600 50 C 450 550 C 3) 3 REFERENCES1)Ministry of Health, Labor and Welfare, ``TheJapanese Pharmacopoeia Fourteenth Edi-tion'', F 114(2001).

9 2)Hirokawa Shoten, ``Dai 14 Kaisei Nihon Yak-kyokuhou Kaisetsusyo'', B 141 2001 3)Society of Japanese Pharmacopoeia, ``TheJapanese Pharmacopoeia Technical Informa-tion,'' 101(2001).4)Japanese Pharmacopoeial Forum,10,135(2001).