顶空气相色谱法测定硫黄熏蒸中药材中二氧化硫的残留量  

Determination of sulfur dioxide residues in sulfur fumigated Chinese herbs with headspace gas chromatography

作　　者：郏征伟[1] 毛北萍[1] 苗水[1] 毛秀红[1] 季申[1] 

机构地区：[1]上海市食品药品检验所,上海201203

出　　处：《药学学报》2014年第2期277-281,共5页Acta Pharmaceutica Sinica

基　　金：科技部重大新药创制资助项目(2009ZX09502-024)

摘　　要：硫黄熏蒸作为一种贮藏养护手段在中药材及其饮片的加工过程中极为常见，该步骤不仅可以促进药材的干燥，同时还能防虫、防霉以及漂白增色等。但熏蒸同时也会引起中药材有效成分的改变，且不规范使用易造成二氧化硫过度残留，对人体健康构成威胁。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·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.

关 键 词：硫黄熏蒸 项空 气相色谱 二氧化硫 

分 类 号：R917[医药卫生—药物分析学]