FEASIBILITY OF DIRECT SOLID SAMPLING FOR ARSENIC DETERMINATION IN SULFUR-CONTAINING ACTIVE PHARMACEUTICAL INGREDIENTS BY GF AAS

E. Flores, F. Duarte, Gabriel T. Druzian, Mariele S. Nascimento, J. Barin, R. Bolzan
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Abstract

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.
gf原子吸收光谱法直接固体进样测定含硫活性药物成分中砷的可行性
建立了直接固体进样石墨炉原子吸收法(DSS-GF原子吸收法)测定含硫原料药中砷的方法。该方法成功地应用于三种sc - api(氢氯噻嗪、呋塞米和磺胺嘧啶)。在热解过程中使用钯和氢作为化学改性剂,可以直接测定sc - api中的as,而不受气态硫的干扰。样品质量(氢氯噻嗪)为0.4 ~ 3mg,用标准水溶液标定是可行的。定量限为0.033 mg g-1,校准范围为0.1 ~ 1.6 ng As。固相样品中直接添加砷的回收率在95 ~ 103%之间,具有良好的准确度。该方法的验证突出了其鲁棒性,因为热解和雾化温度以及Pd和样品质量的变化没有显著改变结果。进一步的实验表明,该方法可应用于其他sc - api(如速尿和磺胺嘧啶)。氢氯噻嗪样品中的砷浓度范围为0.13至0.48 mg g-1,呋塞米和磺胺嘧啶样品中的砷浓度分别为0.49和0.54 mg g-1。使用DSS-GF原子吸收光谱法不需要预先消化样品,可以直接在固体样品中测定砷,具有污染风险低、分析物损失小、准确性好、定量限制等优点。
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