Mass balance method for purity assay of phthalic acid esters: development of primary reference materials as traceability sources in the Japan Calibration Service System

Ishikawa, Keiichiro; Hanari, Nobuyasu; Shimizu, Yoshitaka; Ihara, Toshihide; Nomura, Akihiro; Numata, Masahiko; Yarita, Takashi; Kato, Kenji; Chiba, Koichi

doi:10.1007/s00769-011-0767-0

Cited by 40 publications

(34 citation statements)

References 10 publications

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“…From the results of the purity assay by the freezing point depression method using continuous scan mode, [14][15][16][17] the impurity concentration was obtained to ca. 0.1 mmol mol -1 , and the value was simultaneously consistent with the degree of freezing point depression.…”

Section: Assay For Purity Of Water Used For Certificationmentioning

confidence: 99%

Characterization of Certified Reference Material for the Quantification of Water in Bioethanol

et al. 2012

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The National Metrology Institute of Japan has issued a certified reference material of bioethanol (NMIJ CRM 8301-a) for the quantification of water, methanol, sulfur, and copper. This paper presents technical details for the characterization of the water in NMIJ CRM 8301-a. The characterization was performed using coulometric and volumetric Karl-Fischer (KF) titrations. To reduce moisture absorption, sample handling and KF titration were performed in a glove box under a dried nitrogen atmosphere. In addition, a rubber cap with a three-way valve was attached to the ampoule immediately after opening so as to minimize the influence of moisture. Sample aliquots were obtained using a gas-tight microsyringe through the valve, and injected into the KF cell as soon as possible. The certified value of water obtained from coulometric and volumetric KF titrations was 1.688 mg g -1 , and the expanded uncertainty (coverage factor, k = 2) was 0.028 mg g -1 . This CRM would be suitable for the monitoring of water in bioethanol and similar matrices.

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Section: Assay For Purity Of Water Used For Certificationmentioning

confidence: 99%

Characterization of Certified Reference Material for the Quantification of Water in Bioethanol

et al. 2012

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“…The water mass fraction was determined using a Karl Fischer coulometer (831 model, Metrohm AG, Bleiche West, Switzerland) equipped with a generator electrode without a diaphragm, a current generator electrode (400 mA) and a platinum indicator electrode (10 The volatiles were determined by loss on drying, performed at 60 °C under vacuum for 3 h in case of captopril, at 105 °C for 2 h in case of metronidazole and at 105 °C for 3 h for the other APIs, according to the Brazilian Pharmacopeia IV. 44 The sample amount used per replicate was 0.5 g (Karl Fischer) and 1.0 g (loss on drying).…”

Section: Karl Fischer Coulometric Titration and Loss On Dryingmentioning

confidence: 99%

“…Residual solvents may be introduced in active pharmaceutical ingredients (API) during their synthesis, especially if the final purification step is carried out by crystallization in different solvents, as well as during drug products formulation and manufacturing. 1,7,8 In the particular case of certified reference materials (CRM) of APIs, the determination of volatiles is essential both to demonstrate the compliance with Pharmacopeial acceptance criteria and to allow the mass balance calculation (100% -∑ impurities) [10][11][12] of the API mass fraction. CRMs are produced according to the ISO Guides 34:2009 13 and 35:2006 14 and find application in equipment calibration, method validation and quality control.…”

Section: Introductionmentioning

confidence: 99%

Determination of volatiles in pharmaceutical certified reference materials

Nogueira¹,

Queiroz²,

Silva³

et al. 2012

J. Braz. Chem. Soc.

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Este trabalho compara os resultados obtidos na determinação de voláteis (água e solventes residuais) em novos materiais de referência certificados (MRC) ou candidatos a MRC dos ingredientes ativos farmacêuticos (API) captopril, metronidazol, diclofenaco sódico, diclofenaco potássico e furosemida, através do uso de diferentes técnicas: perda por dessecação (LOD), titulação coulométrica tipo Karl Fisher (KF), cromatografia gasosa (injeção por headspace estático) com detector por ionização em chama (sHS-GC-FID) e com espectrômetro de massas (sHS-GC-MS), análise termogravimétrica (TGA) e espectroscopia no infravermelho próximo (NIR) com análise estatística multivariada dos resultados. As três primeiras técnicas levaram a resultados complementares na determinação de voláteis, enquanto as outras duas mostraram pouca sensibilidade para a determinação de voláteis na faixa de concentração avaliada. A perda por dessecação foi considerada a técnica mais apropriada para determinação da fração mássica de voláteis a ser utilizada no cálculo do teor de API por balanço de massa.This work compares the results obtained for the determination of volatiles (water and residual solvents) in new certified reference materials (CRM) or candidate CRMs of the active pharmaceutical ingredients (API) captopril, metronidazole, sodium diclofenac, potassium diclofenac and furosemide, by means of different techniques: loss on drying (LOD), Karl Fischer (KF) coulometric titration, static headspace gas chromatography with flame ionization detection (sHS-GC-FID) and with mass spectrometry (sHS-GC-MS), thermogravimetric analysis (TGA) and near infrared spectroscopy (NIR) with multivariate chemometric analysis of results. The first three methods led to complementary results. The two other techniques were not sufficiently sensitive to determine volatiles in the concentration range evaluated. The loss on drying method was considered the most appropriate to determine the mass fraction of the volatiles to be used in the mass balance calculation of the API mass fraction in the pharmaceutical CRMs.Keywords: volatiles, water, residual solvents, active pharmaceutical ingredient (API), certified reference materials (CRM), analytical quality control IntroductionSeveral are the reasons for determining the mass fractions of water and residual solvents in pharmaceuticals, including their influence on the physicochemical 1-7 and microbiological stability of raw materials and finished products, their potential toxicity [1][2][3]8 and also economic aspects 9 since their presence results in analyte mass fractions smaller than 100%. Residual solvents may be introduced in active pharmaceutical ingredients (API) during their synthesis, especially if the final purification step is carried out by crystallization in different solvents, as well as during drug products formulation and manufacturing. 1,7,8 In the particular case of certified reference materials (CRM) of APIs, the determination of volatiles is essential both to demonstrate the compliance with Pharmacopeial acc...

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“…Purity (mass fraction) of the principal component can be obtained by subtracting contents of all detected impurities from 100% (kg/kg). 12,13 For this approach, GC-FID or/and high performance liquid chromatography with UV/VIS detector (HPLC-UV) are generally used for the determination of structurally related organic impurities.…”

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confidence: 99%

“…FID detection is known to have a wide dynamic range (10 6 ) and to linearly response to the number of C-H moieties of molecules, approximately equimass response to organic molecules. 12,13 This FID character provides an assumption that peak areas of the principal component and all detected impurities in the material are proportional to their mass fraction in the material. In this respect, GC-FID is widely used as a universal method for the purity assessment of volatile and semi-volatile organic substances.…”

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confidence: 99%

Purity Assessment of Organic Reference Materials with a Mass Balance Method: A Case Study of Endosulfan-II

Kim¹,

Lee²,

Ahn³

et al. 2013

Bulletin of the Korean Chemical Society

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A mass balance method established in this laboratory was applied to determine the purity of an endosulfan-II pure substance. Gas chromatography-flame ionization detector (GC-FID) was used to measure organic impurities. Total of 10 structurally related organic impurities were detected by GC-FID in the material. Water content was determined to be 0.187% by Karl-Fischer (K-F) coulometry with an oven-drying method. Nonvolatile residual impurities was not detected by Thermal gravimetric analysis (TGA) within the detection limit of 0.04% (0.7 µg in absolute amount). Residual solvents within the substance were determined to be 0.007% in the Endosulfan-II pure substance by running GC-FID after dissolving it with two solvents. The purity of the endosulfan-II was finally assigned to be (99.17 ± 0.14)%. Details of the mass balance method including interpretation and evaluating uncertainties of results from each individual methods and the finally assayed purity were also described.

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Mass balance method for purity assay of phthalic acid esters: development of primary reference materials as traceability sources in the Japan Calibration Service System

Cited by 40 publications

References 10 publications

Characterization of Certified Reference Material for the Quantification of Water in Bioethanol

Characterization of Certified Reference Material for the Quantification of Water in Bioethanol

Determination of volatiles in pharmaceutical certified reference materials

Purity Assessment of Organic Reference Materials with a Mass Balance Method: A Case Study of Endosulfan-II

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