分析测试技术与仪器

Research Progress in Analytical Methods of Genetically Modified Organisms

ZHANG Wen-zhu, SHI Jian-hao, XIAO Ming

2015, (4): 191-198.

Abstract(1046)

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Abstract:
By the use of transgenic technology, some of exogenous genes can be transferred into the body of organisms(including animal, plant, and microorganism) and recombine the initial gene of the organism with itself to meet human's various needs, which can eventually produce the so-called genetically modified organisms(GMOs). GMOs a develop rapidly due to their advantages and characteristics. However,with the continuous marketing of transgenic organisms, people hold suspicious and even hostile attitude to their development. The need to monitor and testify the presence and the amount of GMOs in transgenic organisms has boosted various analytical methods for the rapid, effective, accurate and reliable detection of these organisms. In this article the development process, advantages and disadvantages of GMOs, and the urgency to detect and analyze them are introduced. And the recent methods based on DNA, protein, biosensor, and multiple techniques for the detection of genetically modified products are reviewed, and the prospect for the detecting methods of transgenic products in the future is also put forward.

Research Progress of Determination Methods of Zearalenone in Feedsand Foodstuffs

REN Dan-dan, XIE Yun-feng, LI Shao-hui, YANG Yong-tan

2015, (4): 199-204.

Abstract(1011)

PDF(39)

Abstract:
Zearalenone, a secondary metabolite with estrogenic properties, is produced by several Fusarium species that colonize cereal grains. ZEN is hepatotoxic, immunotoxic and genotoxic. It are contaminates foods and feeds wide rangingly, endangers agriculture and pasturage development, and has become a focused point in the field of food safety. In order to effectively control the mycotoxic contamination on grains and grain byproducts, to develop reliable and sensitive determination methods of zearalenone is necessary. In this paper, current laboratory methods to detect ZEN are reviewed.

Problemand Strategy of Flavor Reseach in Aromatic Roasted Peanut Oil

GAO Bei, ZHANG Qing, YANG You-you, YANG Yong-tan

2015, (4): 205-211.

Abstract(1049)

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Abstract:
Aromatic roasted peanut oil(ARPO) which meets the domestic consumers' special expection on sensuous comforts of oil has a great market prospect. In this paper, the existing problem of flavor research in ARPO has been explored and analysed. The present ARPO flavor research deficiency and strategy on accurate quantification, systematically evaluation and formation mechanism were discussed respectively, and the research prospect in this field was proposed.

Determination of Nitrofuran Metabolites in Pork by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

XIE Yun-feng, LI Shao-hui, REN Dan-dan, LIU Jia, AN Xue-jing, YANG Yong-tan

2015, (4): 212-217.

Abstract(1438)

PDF(23)

Abstract:
An analytical method for the determination of 4 nitrofuran metabolites in pork has been developed based on the ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The metabolites in pork samples were hydrolized in hydrochloric acid, and derivatized with 2-nitrobenzaldehyde. After the extraction and concentration with ethyl acetate, the analytes were determined by UPLC-MS/MS in the multiple reaction monitoring mode using an internal standard method. Under the optimized conditions,all the analytes were in good linearity at the range of 0.5~50μg/kg and all the R² were greater than 0.995. The LODs for the metabolites were 0.2μg/kg and the LOQs were 0.5μg/kg.The average recoveries for the blank pork samples at three spiked levels(0.5,1.0 and 10.0μg/kg) ranged from 74.6% to 104.8%,with the relative standard deviations(RSDs, n=6) of 2.4%~15.6%.The proposed method is rapid, accurate and sensitive, and is suitable for the detection of nitrofuran metabolites in pork.

Determination of 7 Artificial Sweeteners in Drink Using Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

LIU Tong, YANG You-you, WANG Hao, MIAO Yu-tian, YANG Yong-tan

2015, (4): 218-224.

Abstract(1202)

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Abstract:
The method for determination of 7sweeteners in wine, grape wine and juice has been developed using the ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) with ammonium acetate solution/methanol as the mobile phase. Prior to centrifuge with 13000 r/min for 10 min, samples were diluted. Under optimized conditions, the limits of detection(LOD, S/N=3) were from 0.003 to 8μg/L and the linear range was between 10 and 500μg/L with R² ≥ 0.9981. Recoveries were in the range of 77.10%~118.94%, and RSDs of the peak areas were between 0.19% and 5.24%. This method is simple, sensitive and reliable, and is suitable for the rapid detection of artificial sweeteners in these three drinks.

Study on Determination of Residual Solvent in Edible Vegetable Oils by Headspace-Gas Chromatography

ZHANG Qing, CHEN Shi-heng, GAO Ding, SHI Xiao-mei, YANG Yong-tan

2015, (4): 225-230.

Abstract(1134)

PDF(37)

Abstract:
A method to determine the residual solvent in edible vegetable oils using headspace-gas chromatography is established. The main components of solvent No.6 were separated completely under the optimized equilibrium temperature and equilibrium time conditions of the headspace auto-sampler.The amount was quantified by an external standard method. The linear relationship was satisfied from 2.0 to 100.0 mg/kg. The average spiked recoveries at three levels were in the range of 98.2%~99.2% and the relative standard deviations(n=6) were less than 2%.With features such as simpleness and accuracy, this method is suitable for the determination of residual solvent in edible vegetable oils.

Rapid Determination of γ-aminobutyric Acid Content in Oolong Tea with Different Fermentation Processes using Automatic Amino Acid Analyzer

MIAO Yu-tian, YANG You-you, LI Song, YANG Yong-tan

2015, (4): 231-235.

Abstract(1112)

PDF(30)

Abstract:
Different fermentation processes will result in different content of γ-aminobutyric acid in tea samples. A method for the determination of γ-aminobutyric acid in Oolong Tea using an automatic amino acid analyzer has been developed, and the trend for the content variation of γ-aminobutyric acid in Oolong Tea using different fermentation processes was investigated. Oolong Tea was soaked for some time, and then determined on a automatic amino acid analyzer. The detection limit of the method was 0.01 g/100g, and the recoveries ranged from 94.4%~109.4%, which meet the requirements of determination. The method with a fast pretreatment procedure has a high throughput and is suitable for the quantitative and qualitative analysis of γ-aminobutyric acid in Oolong Tea, and can be used to investigate different fermentation processes. The determination method is accurate and reliable, which meets the requirements of daily inspection. It also has great significance for the evaluation of the fermentation process whether it can produce high content of γ-aminobutyric acid.

SEM Observation and Analysis of Atmospheric Particulate Matters in Spring Season at Changqing Region

YANG Yong-cheng, ZHANG Xiao-kai, LI Chao-qun, LI Xue, KANG Li-sha

2015, (4): 236-243.

Abstract(1109)

PDF(40)

Abstract:
The microstructure and particle size and distribution of the atmospheric particulate matters were observed in the spring time in Changqing area by use of a scanning electron microscope. The relation curve and histogram of the particle size and distribution of the quantity of atmospheric particulates during a continuous thirty days was drawn using the statistical regression analysis method. The experimental results showed that atmospheric particulates were mainly in a particle size range of 0~1.0μm and 1.0~2.5μm. The microstructure of atmospheric particulate matters included irregular particle, block, spherosome, clava, chip, etc. In addition, the microstructures of Escherichia coli and pollen are observed. The experimental results have reference value to the research of PM2.5 and PM10 in atmosphere and the atmospheric contamination to some extent. And the experimental method is worthy to be applied widely.

Determination of the Migration of Organotin Compounds in Plastic Toys by GC-MS

JIANG Shi-lei, XU Fei-fei, HONG Deng, XIANG Wei, CHEN Ting, ZHU Jun

2015, (4): 244-249.

Abstract(1282)

PDF(25)

Abstract:
A procedure has been developed to determine the migration of organotin compounds in plastic toys by GC-MS method. The organotin compounds were extracted by an 0.07 mol/L hydrochloric acid solution, derivatied with NaBEt4, extracted by hexane, and the quantitative analysis of ethyl organotins was carried out by GC-MS, using an external standard method. The linear calibration curve was obtained in the range of 0.1~7.5 mg/L with a correlation coefficient of >0.9983. The limits of quantification were 0.04~0.16 mg/kg and the average recoveries were in the range of 89.3%~105.4% for 10 organontins with the relative standard deviations <9.7%. The method is simple, rapid, accurate and can be applied to the determination of the migration of orgaontins in plastic toys.

Simultaneous Determination of Five Compounds in Malu Huangxian Mixture by Ultra-High Performance Liquid Chromatography-Photodiode Array Detector

BIAN Meng-yang, LIU Xiao-hua, ZHANG Hai, HAN Zheng-jun, LI Ping, ZHOU Yong-mao, FENG Shi-lan

2015, (4): 250-256.

Abstract(913)

PDF(15)

Abstract:
To a method for the simultaneous quantification of five ingredients in Malu Huangxian Miture is established. Ultra-high performance liquid chromatography-photodiode array detector(UPLC-DAD) was performed on a column of Waters BEH(Φ1.7μm,100 mm×2.10 mm) at the custom wavelengths including 232 nm for 0~3 min, 274 nm for 3~7 min, and at 249 nm for 7~10 min. Methanol-1% acetic acid was used as the mobile phase using gradient elution at a flow rate of 0.61 mL/min. The contents of paeoniflorin, baicalin, baicalein, wogonin and ammonium glycyrrhetate were simultaneously detected by a single injection. Good linear correlation were observed(r=0.9991~0.9999) and the average recovery rates were 99.70%~100.70%. The proved method is simple, accurate, reliable and repeatable that is suitable for the quality control of Malu Huangxian Mixture.

Development of Capillary Electrochromatography Stationary Phases Based Carbon Nanomaterials

RAN Fan-peng, LIU Hong-mei

2015, (4): 257-268.

Abstract(1012)

PDF(21)

Abstract:
Carbon nanomaterials have been widely applied in analytical science, life science, material science, environmental science and other fields due to the unique nano-structure, large specific surface area, strong thermal stability, good electrical conductivity and excellent adsorption properties. In this article, the recent advance of carbon nanomaterials as novel stationary phases of capillary electrochromatography(CEC) in the past five years, including the CEC categories, separation mechanism, preparation methods of chromatographic column and their advantages and disadvantages, structure and properties of carbon nanomaterials(graphene, carbon nanotubes, graphene oxide, reduced graphene oxide, fullerenes), application of carbon nanomaterials as CEC stationary phases and separation mechanisms is reviewed. And the future perspectives of carbon nanomaterials as chromatographic stationary phases are also outlined.

Determination of Manganese,Copper,Lead,Zinc,Chromium and Cadmium in Phosphate Rock by Inductively Coupled Plasma Mass Spectrometry

WANG Jian-bo, CHAI Chang-xin, HUANG Xing-hua, ZHU Jian-guo

2015, (4): 270-273.

Abstract(1100)

PDF(37)

Abstract:
A method for the determination of manganese,copper,lead,zinc,chromium and cadmium in phosphate rock by inductively coupled plasma-mass spectrometry(ICP-MS) is established. The ICP-MS instrument operating parameters were optimized. The mass spectral interferences were eliminated by selecting ⁵⁵Mn,⁶⁵Cu,²⁰⁸Pb,⁶⁶Zn,⁵²Cr and ¹¹⁴Cd as the analytical isotopes. And Rh was selected as the internal standard to compensate the analytical signal drift. Under the optimized conditions with a HNO₃-HClO₄-HF digestion system,the recoveries for these elements were 98.0%~102.0% with a precision of 0.99%~1.98% RSD(n=9).The proposed method has been applied to the determination of these trace heavy metal elements with satisfactory results.

2015 No. 4

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