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Journal of Analytical Methods in Chemistry · 2024 · IF 2.3

Development and Validation of Analytical Procedure for Elemental Impurities in Rosuvastatin Calcium Tablets by ICP-MS and Microwave Digestion

Yajie Hao,Guang Yin,Xuemei Wang,Juan Fu,Qihui Cao,Qinyong Sun,Guimin Zhang,Zhong Feng

Rosuvastatin calcium is a widely used 3-hydroxy-3-methylglutaryl coenzyme A-reductase inhibitor developed for the treatment of dyslipidemia. To establish a control strategy for the elemental impurities, a new digestion method combined with an inductively coupled plasma-mass spectrometer (ICP-MS) was developed and validated by our team to determine elements Cd, Pb, As, Hg, Co, V, and Ni in rosuvastatin calcium tablets, which digest the sample perfectly even in the presence of a large number of excipients, especially titanium dioxide. The measurement mode was collision cell mode with kinetic energy discrimination (KED). 209Bi+, 115In+, and 89Y+ were chosen as internal standard elements. The recoveries of the limit of quantitation (LOQ) ranged from 90.5% to 106.4%, concentrations of the abovementioned elements in LOQ were 0.25 µg·L−1, 0.25 µg·L−1, 0.75 µg·L−1, 1.5 µg·L−1, 2.5 µg·L−1, 5 µg·L−1, and 8 µg·L−1 , respectively, linear correlation coefficients were above 0.9997, the recoveries in accuracy item ranged from 91.8% to 103.6%, and relative standard deviations (RSDs) of recovery in precision were not more than 1.8%, reflecting a reliable method of high sensitivity, strong anti-interference capacity, and good precision, and that it was suitable for the determination of elemental impurities in drugs.

研究领域: 药学 · 分析化学
✓ 已验证 DOI PubMed 高影响因子
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JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY · 2018 ·Vol. 33 ·期 11 ·1910-1916 · IF 3.608

Microwave-induced combustion of graphene for further determination of elemental impurities using ICP-OES and TXRF

Airui Zhang,Hai Wang,Pengfei Zha,Meiling Wang,Haifeng Wang,Bingqi Fan,Danhua Ren,Yanxiang Han,Sitian Gao

An analytical method of microwave induced combustion (MIC) combined with ICP-OES and TXRF is proposed to determine elemental impurities in graphene. Optimized MIC conditions (e.g. sample mass up to 30 mg, microwave irradiation 900 W for 10 min, and oxygen pressure 2 MPa) can achieve the rapid and complete digestion of graphene. Analytical results show that this method can accurately determine elemental impurities such as S, Fe, Cr, Mn and Ni in graphene, and that ICP-OES and TXRF data are comparable. The validity of this method is also verified using three different CRMs for cellulose nanocrystal powder and single-wall carbon nanotubes. The limits of detection (LODs) using MIC combined with ICP-OES are 5.4, 10.6, 7.3, 0.7 and 2.7 μg kg−1 for Fe, S, Cr, Mn and Ni, respectively. The LODs using MIC coupled with TXRF are 30.2, 215, 21.3, 9.5 and 15.8 μg kg−1 for Fe, S, Cr, Mn and Ni, respectively. The experimental results are also compared with those from three other pretreatment methods including dry ashing coupled with acid digestion (DA-AD), microwave-assisted digestion (MWAD) and DA-MWAD, which shows that MIC is superior to the other procedures due to the incomplete digestion and/or escape of volatile S of the latter. The MIC digestion combined with ICP-OES or TXRF could be one of the most promising procedures for the accurate determination of some elemental impurities in carbon nanomaterials with stable structures like graphene.

研究领域: 分析化学 · 材料科学
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Frontiers in Chemistry · 2021 · IF 5.221

Elemental Impurities in Pediatric Calcium Carbonate Preparations-High Throughput Quantification and Risk Assessment

Xiao Chaoqiang,Zhu Li,Zhang Xia,Gao Rumeng,He Shuwang,Lv Zhihua,Hu Changqin

Calcium carbonate which is extracted from the Earth in combination with other mineral impurities, is largely used in preparations for pediatric supplements. Elemental impurities in drug products pose toxicological concerns without therapeutic benefits. Thus, it is very urgent to assess the safety of chronic exposure to elements that may be present in trace amounts. In the present study, we developed high throughput ICP-MS method for the quantitative determination of 62 elemental impurities in high matric calcium carbonate samples and validated according to USP 233. Calcium carbonate preparations which state clearly used for child (including neonates, infants, toddlers and children) from 9 manufactures and two types of raw materials (light calcium carbonate and ground calcium carbonate) were investigated in terms of the content and variability of 62 elemental impurities. According to the results, ground calcium carbonate was more suitable to be used in pediatric preparations concerning elemental impurities. Parts of elemental impurities in CaCO3 preparations which are derived from the raw materials and the preparation process, may cause potential risks for children. These results indicate that it is necessary to establish a modern instrumental analysis method to evaluate and control elemental impurities in CaCO3 raw materials and preparations.

CAS / MDL: 7440-04-2
研究领域: 药学 · 毒理学 · 分析化学
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