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Zhao H.,National Marine Food Quality Supervision and Testing Center | Wang X.,National Marine Food Quality Supervision and Testing Center | Wang X.,Zhejiang Ocean University | Wang P,National Marine Food Quality Supervision and Testing Center | And 3 more authors.
Chinese Journal of Chromatography (Se Pu) | Year: 2013

An analytical method was developed for the determination of the extraetiohof volatile iV-nitrosamine compounds including N-nitrosodimethylamine (NDMA), N-nitrosodiethyl-amine (NDEA), N-nitrosodipropylamine (NDPA), N-nitrosodibutylamine (NDBA), N-nitros-opiperidine (NPIP), and N-nitrosopyrrolidine (NPYE) from salted aquatic products by gas chromatography-mass spectrometry (GC-MS). In thisexperiment, the separation and detection conditions were optimized for different extraction methods, solid-phase extraction columns, and chromatographic columns. The results showed that the linear correlation coefficients (R2 were higher than 0. 999 8 within 10-1 000μg/L. and the reproducibilities were good with the relative standard deviations (RSD) less than 8%. The recoveries were 79%-105%. It is noted that this method for the determination of volatile N-nitrosamine compounds in salted aquatic products was much mor, sensitivity and with a lower detection limits (0. 05 μg/kg except NDPA) than the previously reported methods. This proposed method is rapid and convenient for the determination, and easy for the operation. It is appropriate for the determination of volatile AT-nitroBamine compounds in various salted aquatic products.


Wang P.-Y.,National Marine Food Quality Supervision and Testing Center | Zhou Y.,National Marine Food Quality Supervision and Testing Center | Huang L.,National Marine Food Quality Supervision and Testing Center | Zhao H.,National Marine Food Quality Supervision and Testing Center | And 4 more authors.
Jiliang Xuebao/Acta Metrologica Sinica | Year: 2012

A methd is developed for determination of ampicillin and amoxicillin residues in aquatic product using reversed-phase high performance liquid chromatography-fluorescence detection with pre-column derivatization. The sample extracts are cleaned up by solid-phase extraction cartridge and then derivatized with derivative agent. The results show that the calibration graphs is linear in the concentration rang of 0.001~0.1 mg/kg (r=0.9999). The detection limit and quantification limit are 0.001 mg/kg (S/N=3) and 0.003 mg/kg (S/N=10) for ampicillin, 0.005 mg/kg (S/N=3) and 0.015 mg/kg (S/N=10) for amoxicillin. The average recoveries are between 76.3%~96.8% with relative standard deviations (RSDs) of 0.63%~6.71% (re=6). The method is simple, rapid, sensitive and reproducible, it can be used for the routine analysis of the ampicillin and amoxicillin residues in aquatic product.


Zhao H.,National Marine Food Quality Supervision and Testing Center | Wang X.,National Marine Food Quality Supervision and Testing Center | Wang P.,National Marine Food Quality Supervision and Testing Center | Zhou Y.,National Marine Food Quality Supervision and Testing Center | And 2 more authors.
Se pu = Chinese journal of chromatography / Zhongguo hua xue hui | Year: 2013

An analytical method was developed for the determination of the extraction of volatile N-nitrosamine compounds including N-nitrosodimethylamine ( NDMA) , N-nitrosodiethylamine (NDEA), N-nitrosodipropylamine (NDPA), N-nitrosodibutylamine (NDBA), N-nitrosopiperidine (NPIP), and N-nitrosopyrrolidine (NPYR) from salted aquatic products by gas chromatography-mass spectrometry (GC-MS). In this experiment, the separation and detection conditions were optimized for different extraction methods, solid-phase extraction columns, and chromatographic columns. The results showed that the linear correlation coefficients (R2) were higher than 0. 999 8 within 10 - 1 000 micro g/L, and the reproducibilities were good with the - relative standard deviations (RSD) less than 8%. The recoveries were 79% - 105%. It is noted that this method for the determination of volatile N-nitrosamine compounds in salted aquatic products was much more sensitivity and with a lower detection limits (0. 05 micro g/kg except NDPA) than the previously reported methods. This proposed method is rapid and convenient for the determination, and easy for the operation. It is appropriate for the determination of volatile N-nitrosamine compounds in various salted aquatic products.


PubMed | National Marine Food Quality Supervision and Testing Center
Type: Journal Article | Journal: Se pu = Chinese journal of chromatography | Year: 2010

A novel method was developed for the determination of dichlorobromomethane in water using headspace-trap gas chromatography/mass spectrometry (GC/MS). Three parameters of headspace-trap including thermostatic temperature, time and cycle number were optimized by orthogonal experiment analysis. Dichlorobromomethane in water samples was analyzed under the optimized conditions of 70 degrees C and 20 minutes with the cycle number of two. The results showed that the calibration curve was linear in the range of 0.1 - 10.0 microg/L, and the correlation coefficient was 0.999 1. The detection limit was 0.03 microg/L. The average recovery was 83.1% - 111.3% with the relative standard deviation (RSD) not more than 5.2% (n = 6). This method is rapid, sensitive and reproducible for the routine detection of the low concentration of dichlorobromomethane in water.


PubMed | National Marine Food Quality Supervision and Testing Center
Type: Journal Article | Journal: Se pu = Chinese journal of chromatography | Year: 2010

A method was developed for the determination of 6 p-hydroxybenzoates (methyl p-hydroxybenzoate (MHB), ethyl p-hydroxybenzoate (EHB), isopropyl p-hydroxybenzoate (IPHB), propyl p-hydroxybenzoate (PHB), isobutyl p-hydroxybenzoate (IBHB) and butyl p-hydroxybenzoate (BHB)) in fruits and jams using the combination of solid-phase extraction and high performance liquid chromatography (SPE-HPLC). Two different extraction solutions and three different mobile phases were tested for p-hydroxybenzoates analysis, and finally ethanol was used as the extraction solvent and methanol-citric acid buffer was selected as the mobile phase. The sample was extracted, and purified by an Oasis HLB solid-phase extraction cartridge, then separated on a Symmetry-C18 column and detected at the wave length of 258 nm. The results showed that all the calibration graphs were linear in the concentration range of 0.1 -20.0 mg/L (r = 0.9999). The detection limits and quantification limits were 0.1 mg/kg (S/N = 3) and 0.3 mg/kg (S/N = 10) respectively for MHB, EHB, IPHB and PHB, 0.2 mg/kg (S/N = 3) and 0.6 mg/kg (S/N = 10) respectively for IBHB and BHB. The average recoveries were between 82.8% and 115.5% with the relative standard deviations (RSDs) of 0.2%-6.8% (n = 6). The method is simple, rapid, sensitive and reproducible, and can be used for the routine analysis of the p-hydroxybenzoates in fruits and jams.

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