Determination of Residual Dimethyl Sulfate in Cephalosporin Using HS-SPME/GC-MS.

IF 1.3 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS Journal of chromatographic science Pub Date : 2024-12-11 DOI:10.1093/chromsci/bmae054

Rongchun Lu

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Abstract

Dimethyl sulfate (DMS) is widely used in manufacturing process but because of its genotoxicity nature, it should be monitored at trace levels (1 μg/mL). It is complicated and difficult to quantify DMS in cephalosporin with traditional method. Herein, a method for quantifying residual DMS in cephalosporin was developed, without complex sample preprocessing, no need for a large amount of solvent, employing headspace solid-phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS). Compared with polydimethylsiloxane (PDMS)/divinylbenzene and polyacrylate fibers, PDMS was more suitable for absorbing DMS. The research showed that the PDMS fiber should be changed after 50 adsorption-desorption cycles. Linear regression analysis of the calibration curve demonstrated a robust linear relationship, with R2 of 0.999, across a concentration range of 0.25 to 4.0 μg/mL. The method underwent rigorous validation for specificity, linearity, precision and accuracy. This method was proven effective in measuring DMS in complex matrices. The limits of detection and quantification for this method is 0.05 and 0.25 μg/mL, respectively, which has room for improvement.

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利用 HS-SPME/GC-MS 测定头孢菌素中残留的硫酸二甲酯。

硫酸二甲酯（DMS）在生产过程中被广泛使用，但由于其具有遗传毒性，因此应在痕量水平（1 μg/mL）进行监测。用传统方法定量头孢菌素中的 DMS 既复杂又困难。本文采用顶空固相微萃取（SPME）和气相色谱-质谱联用（GC-MS）技术，建立了一种头孢菌素中残留 DMS 的定量方法，该方法无需复杂的样品预处理，也不需要大量溶剂。与聚二甲基硅氧烷（PDMS）/二乙烯基苯纤维和聚丙烯酸酯纤维相比，PDMS 纤维更适合吸收 DMS。研究表明，PDMS 纤维应在吸附-解吸循环 50 次后更换。校准曲线的线性回归分析表明，在 0.25 至 4.0 μg/mL 的浓度范围内，线性关系良好，R2 为 0.999。该方法在特异性、线性、精密度和准确度方面都经过了严格的验证。该方法被证明可有效测定复杂基质中的 DMS。该方法的检出限和定量限分别为 0.05 和 0.25 μg/mL，还有改进的余地。

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来源期刊

Journal of chromatographic science 化学-分析化学

CiteScore

2.90

自引率

7.70%

发文量

审稿时长

5.6 months

期刊介绍： The Journal of Chromatographic Science is devoted to the dissemination of information concerning all methods of chromatographic analysis. The standard manuscript is a description of recent original research that covers any or all phases of a specific separation problem, principle, or method. Manuscripts which have a high degree of novelty and fundamental significance to the field of separation science are particularly encouraged. It is expected the authors will clearly state in the Introduction how their method compares in some markedly new and improved way to previous published related methods. Analytical performance characteristics of new methods including sensitivity, tested limits of detection or quantification, accuracy, precision, and specificity should be provided. Manuscripts which describe a straightforward extension of a known analytical method or an application to a previously analyzed and/or uncomplicated sample matrix will not normally be reviewed favorably. Manuscripts in which mass spectrometry is the dominant analytical method and chromatography is of marked secondary importance may be declined.