Efficient Determination of Trace Thionyl Chloride in the Antiepileptic Levetiracetam by Pyrolysis Combined with Ion Chro
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ORIGINAL
Efficient Determination of Trace Thionyl Chloride in the Antiepileptic Levetiracetam by Pyrolysis Combined with Ion Chromatography Shaorong Luan1 · Pengyu Liu1 · Fangfang Zhang3 · Lijun Ni1 · Qingchun Huang2 Received: 28 February 2020 / Revised: 14 May 2020 / Accepted: 1 September 2020 / Published online: 18 September 2020 © Springer-Verlag GmbH Germany, part of Springer Nature 2020
Abstract A method involving pyrolysis pretreatment followed by ion chromatography was developed to determine the residual thionyl chloride in levetiracetam. Levetiracetam was combusted at high temperature. After the pyrolysis gas was absorbed, the sulfur in thionyl chloride was converted to sulfate, which were determined by ion chromatography with conductivity detector using potassium hydroxide as the mobile phase. The linearity, limits of detection and quantification, and recovery of the method were evaluated. The average rate of conversion of thionyl chloride to sulfate was 98.2%, indicating good conversion efficiency. The limit of detection for sulfate was 8.85 μg/L. The relative standard deviation of the amount of S OCl2 calculated based on the concentration of sulfate was 2.70%, indicating good repeatability. The recovery for sulfate was 96.0–104%. The results suggest that pyrolysis combined with ion chromatography is an effective method to determine residual thionyl chloride in levetiracetam. Keywords Thionyl chloride · Levetiracetam · Pyrolysis · Ion chromatography
Introduction Epilepsy is a common disease that is widely distributed all over the world [1]. Antiepileptic drugs are generally amide nootropics or cholinergic agonists. To date, antiepileptic drugs such as oxiracetam, aneracetam, praxitan, levetiracetam, neiracetam, and nefexitan have been developed [2]. Among them, levetiracetam is the only antiepileptic drug that has been shown to combine with synaptic vesicle protein SV2A in presynaptic nerve endings, which can inhibit abnormal discharge in the epileptic loop and block the epileptic attack [3]. The antiepileptic effect of levetiracetam is obvious, and the side effects are minor. Levetiracetam can be rapidly and nearly completely (> 95%) absorbed with high * Shaorong Luan [email protected] 1
School of Chemistry and Molecular Engineering, East China University of Science and Technology, Shanghai 200237, China
2
Shanghai Key Lab of Chemical Biology, School of Pharmacy, East China University of Science and Technology, Shanghai 200237, China
3
Thermo Fisher Scientific (China) Co. Ltd., Shanghai 201203, China
bioavailability and a good therapeutic index. Thus, levetiracetam is a widely used and patient-friendly drug, not only for epilepsy, but also with axiolytic activity, distinguishing it from other currently available antiepileptic [4,5]. The preferred route for levetiracetam synthesis in industrialized production is to use l-methionine as starting material to obtain levetiracetam through esterification, amidation, cyclization, and desulfurization methylation, overcomes the major disadva
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