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Zhao Y.,Fuzhou University | Zheng J.,Fuzhou University | Fang L.,Fuzhou University | Lin Q.,Fujian Inspection and Research Institute for Product Quality | And 3 more authors.
Talanta | Year: 2012

A environment-friendly microwave-assisted extraction used to extract trace mercury compounds from fish samples, and a ultra-sensitive method for the analysis of Hg(II), methylmercury (MeHg) and ethylmercury (EtHg) by using capillary electrophoresis-inductively coupled plasma mass spectrometry (CE-ICP-MS) were described in this study. The extraction method is environment-friendly, simple, effective, and can be used to extract trace mercury compounds in fish samples with a satisfied recovery within several minutes. The CE-ICP-MS analytical method has a detection limit as lower as 0.021-0.032 ng Hg/mL for MeHg, EtHg and Hg(II), and can be used to determined ultratrace MeHg, EtHg and Hg(II) in natural water and fish samples directly without any preconcentration. With the help of the above methods, we have successfully determined MeHg, EtHg and Hg(II) in dried fish (Tapertail anchovy) muscle and natural water within 25 min with a RSD (relative standard deviation, n = 6) <5% and a recovery of 94-103%. Our results showed that dried muscle of T. anchovy contained only one species of mercury, MeHg, indicating that MeHg is easier to be accumulated by aquatic organisms. © 2011 Elsevier B.V. All rights reserved.


Xu X.-Q.,Fujian Inspection and Research Institute for Product Quality
Guang Pu Xue Yu Guang Pu Fen Xi/Spectroscopy and Spectral Analysis | Year: 2013

A simple and rapid method for determination of CaO, MgO, Fe2O3, Al2O3 and TiO2 in cement samples by inductive coupled plasma-atomic emission spectrometry (ICP-AES) was developed. In order to carry out the analysis, the cement samples were dissolved with mixed aqua regia, hydrofluoric acid, perchloric acid, hydrochloric acid, and the standard solution was prepared by a series of standard cement samples. The matrix interference and the mutual interference of elements under test were studied by ICP-AES. The detection limits are in the range of 3.79×10-4~1.07×10-2 μg·mL-1. The recovery rates and relative standard deviations (RSD) of the method are in the range of 87.5%~105.6% and less than 1% respectively. Research results show that the method can meet the requirements of rapid chemical analysis for cement.


Lin Q.,Fujian Inspection and Research Institute for Product Quality
Se pu = Chinese journal of chromatography / Zhongguo hua xue hui | Year: 2013

An improved method has been developed for the determination of clavulanate potassium, tazobactam and sulbactam in dairy products. High performance liquid chromatography with photodiode array detector (HPLC-PAD) was used in this method. The separation was performed on a CAPCELL PAK MG-C18 column (150 mm x 4.6 mm, 5 microm). The mobile phase was 0.03% (volume fraction unless otherwise specified) phosphate-acetonitrile. This method offered effective sample preparation procedures including dissolution with water, protein isolation with acetone, clean-up and enrichment by solid-phase extraction (SPE) with PWAX cartridges (60 mg/3 mL) under weak acidic condition and further elution with 0.05% ammonia-methanol solution. The analytical method was well validated and good results were obtained with the RSDs of 2.2% - 7.4% and the recoveries of 84.6% - 101.7%. The detection limits of clavulanate potassium, tazobactam and sulbactam were 0.03 mg/L. All of the target compounds exhibited good linearities (r > 0.999) over the mass concentration range of 0.05 - 5 mg/L. With the advantages of good purification effect, high sensitivity, good recovery and repeatability, the method is suitable for the detection of beta-lactamase inhibitors in dairy products.


Peng K.,Fuzhou University | Mou X.,Fujian Inspection and Research Institute for Product Quality
Jinshu Rechuli/Heat Treatment of Metals | Year: 2013

Cu-35Zn alloy was deformed by ten passes constrained groove pressing (CGP) firstly, and then by cold rolling with 10%-30% strain. The microstructure and properties of Cu-35Zn alloy after processed by CGP and cold rolling were studied. The results show that the grains of Cu-35Zn alloy get fined after CGP. The number of deformation twins in the sample increases and the homogeneity of the sample is also improved by subsequent cold rolling. With the increasing of cold rolling strain, the hardness and strength of Cu-35Zn alloy after the deformation of CGP plus cold rolling are increased, but the elongation decreases.


Lin Q.,Fujian Inspection and Research Institute for Product Quality
Chinese Journal of Chromatography (Se Pu) | Year: 2013

An improved method has been developed for the determination of clavulanate potassium, tazobactam and sulbactam in dairy products. High performance liquid chromatography with photodiode array detector (HPLC-PAD) was used in this method. The separation was performed on a CAPCELL PAK MG-C18 column (150 mm x 4.6 mm, 5 μm). The mobile phase was 0.03% (volume fraction unless otherwise specified) phosphate-acetonitrile. This method offered effective sample preparation procedures including dissolution with water, protein isolation with acetone, clean-up and enrichment by solid-phase extraction (SPE) with PWAX cartridges (60 mg/3 mL) under weak acidic condition and further elution with 0.05% ammonia-methanol solution. The analytical method was well validated and good results were obtained with the RSDs of 2.2% - 7.4% and the recoveries of 84.6% - 101.7%. The detection limits of clavulanate potassium, tazobactam and sulbactam were 0. 03 mg/L. All of the target compounds exhibited good linearities (r > 0.999) over the mass concentration range of 0. 05 - 5 mg/L. With the advantages of good purification effect, high sensitivity, good recovery and repeatability, the method is suitable for the detection of β-lactamase inhibitors in dairy products.


You F.,Fujian Inspection and Research Institute for Product Quality
Chinese Journal of Chromatography (Se Pu) | Year: 2015

A sensitive method was developed for the simultaneous determination of six components which included 4,4′-diaminodiphenylamine sulfate hydrate and 2,4-diaminophenol sulfate, etc. in hair dyes by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). After extracted by water through ultrasonic extraction, the samples were analyzed by UPLC-MS/MS. The separation was performed on a Waters BEH-C18 column (100 mm × 2.1 mm, 1.7 μm) with gradient elution of 10 mmol/L ammonium acetate and acetonitrile. The electrospray ionization (ESI) source in positive ion mode was used for the analysis of the six components in the multiple reaction monitoring (MRM) mode. The results showed good linear relationships with all the correlation coefficients (R2) more than 0.99. The limits of detection (LODs, S/N = 3) for the six components were in the range of 0.26-4.6 mg/kg. The average recoveries of the six components in the spiked samples were in the range of 83.0%-92.2% with the relative standard deviations (RSDs, n=6) of 5.4%-11.2%. The precision, accuracy, mean recoveries and the matrix effects satisfied the requirements of cosmetic sample measurement. The proposed method has been applied to the determination of six dyes in actual samples. This method is simple, accurate and effective for the simultaneous determination of the six components in hair dyes.


Wang Z.,Fujian Inspection and Research Institute for Product Quality
Chinese Journal of Chromatography (Se Pu) | Year: 2012

A confirmatory method is presented for the determination of five nitro-musks (musk ambrette, musk xylene, musk moskene, musk tibeten and musk ketone) in different cosmetics by gas chromatography coupled with negative chemical ionization (NCI)-triple quadrupole mass spectrometry (GC-MS / MS). The samples were extracted under ultrasonication using a mixture of acetone and hexane. The extract was concentrated and then cleaned up by CNWBOND Si solid phase extraction cartridge. Five different instrument parameters such as the temperature programmed, ion source temperature, reagent gas pressure, collision energy, monitoring ion pairs were optimized for higher sensitivity. Then the analytes were qualitatively and quantitatively analyzed under the multiple reaction monitoring (MRM) mode after the chromatographic separation on an HP-5MS capillary column (30 m × 0 25 mm, 0 25 μm), and employing d15-musk xylene as internal standard. The mixed standards were spiked in the blank cosmetics samples (each nitro-musk was about 500 ng / kg), and the recoveries were in the range of 85 81% -103 77% with the relative standard deviations (RSDs) not more than 5 32%. The limits of quantification of the method were about 50 0 -500 ng / kg. The method is accurate, rapid, sensitive and can be used in the inspection of the five nitro-musks in cosmetics.


Yuan C.,Chinese Academy of Sciences | Liu B.,Chinese Academy of Sciences | Liu F.,Fujian Inspection and Research Institute for Product Quality | Han M.-Y.,Institute of Materials Research and Engineering of Singapore | Zhang Z.,Chinese Academy of Sciences
Analytical Chemistry | Year: 2014

A new "turn on" fluorescence nanosensor for selective Hg 2+ determination is reported based on bis(dithiocarbamato)copper(II) functionalized carbon nanodots (CuDTC2-CDs). The CuDTC2 complex was conjugated to the prepared amine-coated CDs by the condensation of carbon disulfide onto the nitrogen atoms in the surface amine groups, followed by the coordination of copper(II) to the resulting dithiocarbamate groups (DTC) and finally by the additional coordination of ammonium N-(dithicarbaxy) sarcosine (DTCS) to form the CuDTC2-complexing CDs. The CuDTC 2 complex at surface strongly quenched the bright-blue fluorescence of the CDs by a combination of electron transfer and energy transfer mechanism. Hg2+ could immediately switch on the fluorescence of the CuDTC 2-CDs by promptly displacing the Cu2+ in the CuDTC 2 complex and thus shutting down the energy transfer pathway, in which the sensitive limit for Hg2+ as low as 4 ppb was reached. Moreover, a paper-based sensor has been fabricated by printing the CuDTC 2-CDs probe ink on a piece of cellulose acetate paper using a commercial inkjet printer. The fluorescence "turn on" on the paper provided the most conveniently visual detection of aqueous Hg2+ ions by the observation with naked eye. The very simple and effective strategy reported here facilitates the development of portable and reliable fluorescence nanosensors for the determination of Hg2+ in real samples. © 2013 American Chemical Society.


Zhang K.,Chinese Academy of Sciences | Yu T.,CAS Institute of Chemistry | Liu F.,Fujian Inspection and Research Institute for Product Quality | Sun M.,Chinese Academy of Sciences | And 5 more authors.
Analytical Chemistry | Year: 2014

Semiconductor nanocrystals (NCs) possess unique photoluminescent properties which can be used to design fluorescence probes for chemo/biosensing applications. Several have recently emerged that offer excellent turn-on or ratiometric fluorescence chemosensory protocols by sophisticated procedures, but it has been challenging to realize all of these advantages in a single construct. Herein, we develop an intrinsic dual-emitting Mn-doped ZnS nanocrystal-based probe that achieves this goal with turn-on and ratiometric fluorescence response for the determination of organophosphate (diethylphosphorothioate, DEP). The probe relies on the modification of dopamine dithiocarbamate on the surface of NCs and the modulation of dual emission through a photoinduced electron transfer process, which makes use of red fluorescence of Mn2+ ions doped in the NCs as specific recognition for the target analyte and blue defect emission of the NCs as stable internal reference. In presence of DEP, the red emission of the probe is thus enhanced by switching off the electron transfer pathway, while the blue emission is almost unchanged. With the addition of different amounts DEP, the two emission intensity ratios gradually vary and display color changes from dark-blue to purple to red. Thus, this method generates turn-on and ratiometric fluorescence signals for quantitative and visual detection of the analyte. Significantly, the dual-emitting probe has been used to fabricate paper-based test strips for visual detection of DEP residues, which validate the method for its rapid, on-site, and visual identification. © 2014 American Chemical Society.


Huang Y.,Fujian Inspection and Research Institute for Product Quality
Chinese Journal of Chromatography (Se Pu) | Year: 2011

A comprehensive analytical method based on ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) has been developed for the determination of virginiamycin M 1 in feeds. The sample was extracted twice by ultrasonic extraction with acetonitrile-0.2% (v/v) formic acid (8:2, v/v). The chromatographic separation was achieved with a BEH C18 column and acetonitrile-0.3%(v/v) formic acid (35:65, v/v) as the mobile phase. The identification and quantification of the analyte were carried out on electrospray ionization MS/MS in a multiple reaction monitoring (MRM) mode. The correlation coefficient ® of virginiamycin M1 was 0.9995 in the linear range of 0.3~226.6 μg/L. The detection limit (S/N=3) and quantification limit (S/N=10) of virginiamycin M1 were 2 μg/kg and 7 μg/kg, respectively. The average spiked recoveries were in the range of 82.6% to 102.7% with the relative standard deviations (RSDs) of 0.9%~10.5%. The results demonstrate that the proposed method is simple, sensitive, repeatable and suitable for the testing of virginiamycin M 1 in feeds.

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