Jia Zheng-Wei, Mao Bei-Ping, Miao Shui, Mao Xiu-Hong, Ji Shen
Yao Xue Xue Bao. 2014 Feb;49(2):277-81.
This paper aims to establish a method for the determination of sulfur dioxide in sulfur fumigation Chinese herbs. Sample powder and hydrochloric acid solution were isolated by paraffin layer in order to avoid early reactions, with the generation of sulfur dioxide, headspace with airtight needle was used to transfer sulfur dioxide into gas chromatograph, and detected with thermal conductivity detector. The analytical performance was demonstrated by the analysis of 12 herbs, spiked at four concentration levels. In general, the recoveries ranging from 70% to 110%, with relative standard deviations (RSDs) within 15%, were obtained. The limit of detection (LOD) was below 10 mg x kg(-1). Standard addition can be used for low recovery samples. The method is simple, less time-consuming, specific and sensitive. Methods comparison revealed that gas chromatography is better than traditional titration in terms of method operability, accuracy and specificity, showing good application value.
本文旨在建立一种测定硫磺熏蒸中药材中二氧化硫的方法。样品粉末和盐酸溶液通过石蜡层分离以避免过早反应生成二氧化硫,采用气密针将顶空中的二氧化硫转移至气相色谱仪中,并用热导检测器进行检测。通过对12种草药在四个浓度水平下加标分析来证明该分析性能。总体而言,回收率在70%至110%之间,相对标准偏差(RSD)在15%以内。检测限(LOD)低于10 mg·kg⁻¹。对于回收率低的样品可采用标准加入法。该方法简便、耗时少、特异性强且灵敏。方法比较表明,气相色谱法在方法可操作性、准确性和特异性方面优于传统滴定法,具有良好的应用价值。