scholarly journals Determination of eight kinds of glucocorticoids residues in chicken muscle with on-line clean up combined HPLC-MS/MS

2021 ◽  
Author(s):  
Yahua Yang ◽  
Zhizhong Xue ◽  
Ran Meng ◽  
Zhe Wu ◽  
Zhaojia Li ◽  
...  
Keyword(s):  
Solid Phase ◽  
Sample Pretreatment ◽  
Extraction Column ◽  
Spectral Parameters ◽  
Mass Spectral ◽  
Chicken Muscle ◽  
On Line ◽  
Pretreatment Conditions ◽  
Selective Analysis

AbstractA sensitive and rapid method using HPLC-MS/MS was developed for the determination of eight glucocorticoids residues in chicken muscle simultaneously by Turbo Flow. The eight glucocorticoids were prednisone, prednisolone, hydrocortisone, methylprednisolone, dexamethasone, betamethasone, beclomethasone and fludrocortisones. Samples were extracted with ethyl acetate and on-line cleaned up through a Turbo Flow solid-phase extraction column without time-consuming pretreatment before HPLC-MS/MS analysis. Sample pretreatment conditions, Turbo Flow conditions and mass spectral parameters were optimized and obtained eight glucocorticoids calibration curves. These curves showed good linearity over the concentration from 0.2 μg/kg to 50 μg/kg with an average recovery from 71.63% to 117.36%. This method could be applied on real samples and provided simple, rapid, sensitive and highly selective analysis, which made it feasible to be adopted in food inspection organizations or carry out quantitative analysis for other banned substance.

Determination of Streptomycin and Dihydrostreptomycin in Animal Tissue by On-Line Sample Enrichment Liquid Chromatography

1994 ◽  
Vol 77 (2) ◽  
pp. 334-337 ◽  
Author(s):  
Geoff C Gerhardt ◽  
Craig D C Salisbury ◽  
James D MacNeil
Keyword(s):  
Solid Phase ◽  
Animal Tissue ◽  
Extraction Column ◽  
Chromatographic System ◽  
Perchloric Acid Solution ◽  
Sample Enrichment ◽  
On Line ◽  
Liquid Chromatographic ◽  
Line Sample

Abstract A method for the determination of streptomycin and dihydrostreptomycin in pork and bovine muscle and kidney was developed. Dilute perchloric acid solution is used to precipitate proteins and extract the analytes from the tissue. The extract is loaded onto a cation-exchange, solid-phase extraction column, and the drugs are eluted with pH 8 phosphate buffer. The eluant is chromatographed by using an on-line column enrichment liquid chromatographic system with postcolumn derivatiza-tion using 1,2-naphthoquinone-4-sulfonic acid and detection by fluorescence. The recoveries were 61.1% (coefficient of variation [CV], 7.3%) for streptomycin and 55.3% (CV, 8.2%) for dihydrostreptomycin. The detection limits were 10 ppb for streptomycin and 20 ppb for dihydrostreptomycin.

scholarly journals Determination of Aflatoxin Bi in Pistachio Kernels and Shells

1996 ◽  
Vol 79 (6) ◽  
pp. 1360-1364 ◽  
Author(s):  
Jos M Scholten ◽  
Martien C Spanjer
Keyword(s):  
Aflatoxin B1 ◽  
Solid Phase ◽  
Tolerance Limit ◽  
Extraction Column ◽  
Phase Extraction ◽  
Entire Sample ◽  
Edible Portion ◽  
Pistachio Nuts ◽  
On Line

Abstract A method was developed for accurate measurement of aflatoxin B1 in the edible portion of pistachio nuts. Twenty-nine samples of kernels with and without their shells were slurried with a Mega Ultra Turrax. A subsample of the homogenate was extracted with water–methanol, defatted with petroleum ether, purified with a silica solid-phase extraction column, and redissolved in methanol. After separation on an octadecy! column and postcolumn reaction with on-line electrochemically generated bromine, the aflatoxin Bi derivative was detected fluorometrically. The shells contained less than 1 % of the aflatoxin Bi found in the edible kernel, and they accounted for 41.7–46.8% of the weight of the whole pistachio. These observations indicate it is possible to analyze an entire sample, up to 25 kg, as a whole and still be able to judge whether it meets the legal tolerance limit of 5 μg aflatoxin B1/kg edible part, as set by the Dutch Food Act.

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