Determination of toxic elements in tricyclic active pharmaceutical ingredients by ICP-MS: a critical study of digestion methods

Barin, Juliano S.; Tischer, Bruna; Picoloto, Rochele S.; Antes, Fabiane Goldschmidt; Silva, Fabiana E. B. da; Paula, Fávero Reisdorfer; Flores, Érico M.M.

doi:10.1039/c3ja50334h

Cited by 37 publications

(9 citation statements)

References 21 publications

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“…The proposed method by DSS-GF AAS for As determination in SC-APIs presented similar LOQ to those found in literature for other APIs using ICP-MS after sample digestion (MIC/wet digestion) [13,31]. However, DSS-GF AAS allowed the use of lower sample amounts (<3mg), contrarily to other methods that required previous sample digestion of higher sample amounts (from 80 up to 500 mg) [13,31]. In addition, the time-consuming sample preparation step and the use of concentrated reagents (i.e.…”

supporting

confidence: 77%

“…As also observed for hydrochlorothiazide samples, the arsenic concentrations were not statistically different from those by ICP-MS and GF AAS after acid digestion and the results by ICP-OES were lower than the LOD. The proposed method by DSS-GF AAS for As determination in SC-APIs presented similar LOQ to those found in literature for other APIs using ICP-MS after sample digestion (MIC/wet digestion) [13,31]. However, DSS-GF AAS allowed the use of lower sample amounts (<3mg), contrarily to other methods that required previous sample digestion of higher sample amounts (from 80 up to 500 mg) [13,31].…”

supporting

confidence: 73%

“…However, before the determination by ICP-OES or ICP-MS, the solubilization or digestion of sample matrix is commonly performed by using concentrated acids and under heating [4,10]. Unfortunately, this procedure generally is time consuming and prone to contamination and analyte losses [12][13][14]. On the other hand, As can also be determined by graphite furnace atomic absorption spectrometry (GF AAS), a wellestablished technique for As determination in several types of samples [15][16].…”

Section: Introductionmentioning

confidence: 99%

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Feasibility of Direct Solid Sampling for Arsenic Determination in Sulfur-Containing Active Pharmaceutical Ingredients by Gf Aas

et al. 2019

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A method for As determination in sulfur-containing active pharmaceutical ingredients (SC-APIs) by direct solid sampling graphite furnace atomic absorption (DSS-GF AAS) was developed. The proposed method was successfully applied to three SC-APIs (hydrochlorothiazide, furosemide and sulfadiazine). Palladium was used as chemical modifier as well as hydrogen during the pyrolysis allowing the direct determination of As in the SC-APIs without interferences caused by gaseous sulfur species. Sample masses (hydrochlorothiazide) from 0.4 to 3 mg were used and calibration with aqueous standard solutions was feasible. The limit of quantification was 0.033 mg g-1 and the calibration ranged from 0.1 to 1.6 ng As. Recoveries for As solutions added directly to the solid samples were between 95 and 103%, showing a good accuracy. The method validation highlighted its robustness, since variation in pyrolysis and atomization temperatures, as well as in Pd and sample masses, did not change significantly the results. Additional experiments showed that this method can be applied to other SC-APIs (as e.g., furosemide and sulfadiazine). Arsenic concentration in hydrochlorothiazide samples ranged from 0.13 to 0.48 mg g-1, while in furosemide and sulfadiazine samples it was from 0.49 and 0.54 mg g-1, respectively. The use of DSS-GF AAS does not require previous sample digestion and As could be directly determined in the solid samples providing some advantages, as lower risks of contamination and analyte losses, good accuracy and limits of quantification.

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supporting

confidence: 77%

supporting

confidence: 73%

Section: Introductionmentioning

confidence: 99%

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Feasibility of Direct Solid Sampling for Arsenic Determination in Sulfur-Containing Active Pharmaceutical Ingredients by Gf Aas

et al. 2019

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“…wave atomic absorption spectroscopy (AAS), gas chromatography-mass spectroscopy (GC-MS), inductively coupled plasma mass spectroscopy (ICP-MS), and highperformance liquid chromatography (HPLC) (Puk and Weber 1994;Vallant et al 2007;Barin et al 2014;Han et al 2006). However, these techniques are highly expensive, and require sophisticated operating facilities, complex sample treatments and skilled personnel, and thus are not suitable for field deployment.…”

Section: Introductionmentioning

confidence: 99%

Dual mechanism-based sensing of mercury using unmodified, heteroepitaxially synthesized silver nanoparticles

et al. 2017

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Mercury and its compounds are widely distributed in the environment and have a significant negative impact on human health. In this paper, we report the development of a rapid and facile method for the detection of mercury ions (Hg 2? ) using heteroepitaxially synthesized unmodified silver nanoparticle-based smart probes using UV-Vis spectrophotometer and also through the naked eye by means of a paper-based sensor strip. The silver nanoparticles were prepared by heteroepitaxial growth method using gold seed nanoparticle of *2.4 nm size as the template. The silver is grown on the seed particles by reducing the silver-ammonia complex using glucose, which resulted in Glu-AgNPs having an average size of 14.65 ± 3.53 nm. The sensing of mercury ions was carried out in aqueous solution and the reaction response was monitored by UV-Vis spectrophotometer. The interaction of Hg 2? with Glu-AgNPs resulted in a significant drop in the absorbance at 402 nm along with a prominent color change (from bright yellow to colorless) and wavelength shift (blue shift). The limit of detection (LOD) of this assay was found to be 100 nM (i.e., 20 ppb) with a good linearity in the concentration range of 100-10 mM. To further ease the detection process and make it field deployable, we attempted to develop a paper-based sensor strip by immobilizing Glu-AgNPs on a paper strip. Upon interaction with mercury solution of varying concentrations, the decoloration of the spots could be observed easily through naked eyes, with the limit of detection under sub-optical conditions being 1 lM.

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“…Numerous methods to analyze various elements have been reported. [6][7][8][9][10][11][12] Inductivity coupled plasma atomic (optical) emission spectroscopy (ICP-AES or ICP-OES) and inductivity coupled plasma mass spectrometry (ICP-MS) are described in USP chapter (233). ICP-MS is one of the most effective methods to determine the concentrations of metal elements because the ICP-MS can detect extremely low-level metal concentrations even below those required by the regulations.…”

Section: Introductionmentioning

confidence: 99%

Stabilizers for Osmium Isotopes in Microwave-Irradiated Acid Digestion and Inductively Coupled Plasma Mass Spectrometry Analysis

Takayama

Yoneda

Takebayashi

et al. 2022

CHEMICAL & PHARMACEUTICAL BULLETIN

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Osmium is defined in the international council for harmonization (ICH-Q3D) guidelines as an element whose concentration can be determined by validated methods including microwave-assisted nitric acid digestion and inductively coupled plasma mass spectrometry. However, microwave digestion using nitric acid is known to result in osmium recoveries higher than the theoretical values in spiked tests because of the formation of highly volatile osmium tetroxide in an oxidation reaction. To stabilize osmium, the addition of thiourea as a complexing agent has been tested and proved its utility. It remains unclear whether other compounds can prevent the over-recovery of osmium. In this study, we investigated four compounds, thiourea, ascorbic acid, sodium sulfite, and potassium metabisulfite, that could reduce the overestimation of osmium isotopes. The minimum amounts of thiourea, ascorbic acid, sodium sulfite, and potassium metabisulfite required to stabilize 10 ng/mL osmium in blank matrix were 1.0, 1.0, 2.5, and 2.5 g/L, respectively. The relative standard deviations obtained from 12 analyses for each stabilization solution were less than 3.3% in thiourea, 12.7% in ascorbic acid, 9.0% in sodium sulfite, and 10.6% in potassium metabisulfite. The stabilization solutions were investigated in a digested tablet matrix and were found to be effective. The impact of adding stabilization solutions on the determination of all ICH-Q3D element concentrations was also evaluated. As stabilization solutions had a small or significant impact on the determination of some elements, it was concluded that osmium determination should be conducted independently.

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Determination of toxic elements in tricyclic active pharmaceutical ingredients by ICP-MS: a critical study of digestion methods

Cited by 37 publications

References 21 publications

Feasibility of Direct Solid Sampling for Arsenic Determination in Sulfur-Containing Active Pharmaceutical Ingredients by Gf Aas

Feasibility of Direct Solid Sampling for Arsenic Determination in Sulfur-Containing Active Pharmaceutical Ingredients by Gf Aas

Dual mechanism-based sensing of mercury using unmodified, heteroepitaxially synthesized silver nanoparticles

Stabilizers for Osmium Isotopes in Microwave-Irradiated Acid Digestion and Inductively Coupled Plasma Mass Spectrometry Analysis

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