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1.
Yao Xue Xue Bao ; 49(2): 277-81, 2014 Feb.
Article in Chinese | MEDLINE | ID: mdl-24761623

ABSTRACT

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.


Subject(s)
Chromatography, Gas/methods , Fumigation , Plants, Medicinal/chemistry , Sulfur Dioxide/analysis , Limit of Detection , Sulfur/chemistry
2.
Yao Xue Xue Bao ; 45(3): 353-8, 2010 Mar.
Article in Chinese | MEDLINE | ID: mdl-21351512

ABSTRACT

The paper is to report the establishment of a method for the determination of multi-residue organochlorine and pyrethroid pesticides in traditional Chinese medicines (TCMs). Fifty-six pesticides were extracted by high-speed homogenization, and then purified through gel permeation chromatography (GPC) and solid phase extraction (SPE) cartridges. The residues were simultaneously identified and quantified by GC-ECD equipped with dual tower, dual column and two micro-ECD detectors. The analytical performance was demonstrated by the analysis of 3 TCMs samples' extracts, spiked at three concentration levels for each pesticide. In general, the recoveries ranging from 70% to 110%, with relative standard deviations (RSDs) better than 15%, were obtained. The limit of detection (LOD) for most of the targeted pesticides tested was below 0.01 mg kg(-1). The method had good extraction efficiency, purification effect and good reproducibility, which could be applied to the determination of organochlorine and pyrethroid pesticide residues in the routine analysis of TCMs.


Subject(s)
Drug Contamination , Drugs, Chinese Herbal/chemistry , Hydrocarbons, Chlorinated/analysis , Pesticide Residues/analysis , Pyrethrins/analysis , Chromatography, Gas/methods , Chromatography, Gel , Limit of Detection , Reproducibility of Results , Solid Phase Extraction
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