分析测试技术与仪器

Application of 1-ehenyl-3-Methylimidazolium Iodide Ionic Liquid/Molecularly Imprinted Materials in Recognition of Bovine Hemoglobin

CHEN Yi-ting

2018, 24(1): 1-6. doi: 10.16495/j.1006-3757.2018.01.001

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The molecularly imprinted polymers are macromolecular adsorbing materials with specific discrimination for target molecules. Using bovine hemoglobin (BHb) as the template molecule, acrylamide and the ionic liquid 1-vinyl-3-methylimidazolium iodide were polymerized under the functions of the cross-linking agent, initiator and accelerator by a bulk polymerization. The molecularly imprinted materials prepared have a specific recognition for BHb. The recognition conditions were optimized and discussed.

Risk Assessment of Pb, Cd in Melamine Tableware

YU Xiu-juan, YANG Tian-yu, FAN Ji-peng, ZHU Zhen-hua, GU Juan-hong

2018, 24(1): 7-11. doi: 10.16495/j.1006-3757.2018.01.002

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The migration regularities of lead and cadmium in melamine tableware were investigated. The safety risk assessment of lead and cadmium in melamine tableware were studied, and the suggested values of lead and cadmium in melamine tableware were put forward to protect the safety and health of people.

Adsorption and Separation of Non-Steroidal Anti-Inflammatory Drugs

WANG Xiao-qi, LIU Hong-mei

2018, 24(1): 12-22. doi: 10.16495/j.1006-3757.2018.01.003

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Non-steroidal anti-inflammatory drugs(NSAIDs) are widely used in the treatment of human diseases because of their good anti-inflammatory, antipyretic and analgesic effects. These non-steroidal drugs that entered the human body cannot completely be metabolized by the liver during the treatment of inflammation and the rest of its metabolites excreted through the excretory system of body. Large amounts of data indicate that the residual drugs in the environment are directly or indirectly presented as food safety problems, therefore it becomes one of the main investigations in many fields, such as analytical chemistry and material chemistry. Sample pretreatment techniques are frequently used to carry out the adsorption and separation analysis due to the complexity of the sample matrix, the wide range of analytical components and the low content of the target analyte. In recent years the problems caused by non-steroidal anti-inflammatory drugs and the variety of analysis of the separation and detection techniques of the non-steroidal anti-inflammatory drugs mechanism for the environment are summarized. The core of separation and determination is the selection of extracting materials. The research progress on non steroidal anti-inflammatory drugs for the effective, outstanding adsorption and separation of materials are reviewed.

Determination of Phthalates Contaminants in Health Care Wine by Gas Chromatography-QQQ Mass Spectrometry

MA Chun-yan, LU Qie-nan, DUAN Qiong, HU Wei-jie, FENG Shu-hua, LIU Xue-li

2018, 24(1): 23-27. doi: 10.16495/j.1006-3757.2018.01.004

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A method for the determination of 16 phthalates in the health care wine by gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS) was developed. Pretreatment methods of phthalate esters in health care wine were studied and optimized. An extraction method to remove ethanol on a boiling water bath was established, using n-hexane as the extractant. Quantitative analysis was performed on the time selective reaction scanning mode (T-SRM). The chromatographic column used was a TG-5MS quartz capillary column (30 m×0.25 mm×0.25 μm), the programmed temperature (initial column temperature was 60℃, kept for 1 min, and raised to 220℃ at 20℃/min, kept for 1 min, then kept at 5℃/min to 280℃, kept for 4 min), without shunting. The results showed that the 16 phthalates had an effective internal correlation (R² > 0.995). The average recovery was 84.0%~112.8%, and the RSD was less than 7% (n=6). 6 PAEs in health care wine were determined by this method. The results showed that the method is sensitive, simple and rapid, accurate and reliable. The GC-MS/MS method can satisfy the qualitative analysis and quantitative determination of the phthalates in health care wine.

Simultaneous Determination of 10 Dye Components in Hair Dye by High Performance Liquid Chromatography

WANG Hai-rui, CHEN Shao-bo, XU Zhen-dong

2018, 24(1): 28-33. doi: 10.16495/j.1006-3757.2018.01.005

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In this article a simultaneous analytical method for the detection of P-phenylene diamine and other 10 oxidation type dye components in hair dye by high performance liquid chromatography is described. The objectives of dye derivatives p-phenylenediamine, resorcine, p-aminopheno, m-aminophenol, 4-amino-m-cresol, hydroquinone, 4-amino-2-hydroxytoluene, p-diamino-2-nitrobenzene, 2, 5-diaminotoluene sulfate, 6-hydroxyindole were seperated on a Poroshell 120 Bonus-RP capillary column. Mass spectrometry was used to quantify the dye in hair dye. Results showed that correlation coefficients of the method were from 0.999 85 to 0.999 96. The relative standard deviation(RSD) was less than 5.91% when the concentrations were in the range of 0.01~0.5 mg/mL, the recovery was from 87.2% to 106.7%. The determination results demonstrated that the method had the feature of simple, rapid, and higly selective.

Analysis of Five Hypnotic Sedative Drugs in Blood by Gas Chromatography-Mass Spectrometry with Supported Liquid Extraction

LI Wen-hai, LI Xiu-yun, LIN Da-wei, SUN Hong-lei, SHAO Kai

2018, 24(1): 34-38. doi: 10.16495/j.1006-3757.2018.01.006

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To establish a gas chromatography-mass spectrometry(GC/MS) method with supported liquid extraction(SLE) for the determination of common sedative hypnotic drugs in blood. Five sedative hypnotic drugs, amitriptyline, estazolamum, midazolam, promethazine and chlorpromazine, were determined by GC/MS after being processed with SLE, and experimental conditions were optimized. After adding five sedative hypnotic drugs in the blank blood, they were separated and determined by SLE-GC/MS. Optimal experimental conditions were:pH 10 and 5.0 mL of ethyl acetate as the extraction solvent. The results showed a good linearity among the concentrations of 0.5~20 μg/mL of the five drugs and the peak areas with correlation coefficients of 0.998 1~0.999 5, the limits of quantification(LOQ) were approximately 0.5 μg/mL, the average recoveries were 70.1%~90.8%, and the coefficient of variation was less than 5. 3%. The method is simple, rapid, with a high recovery, and it can be used in the determination of common sedative hypnotic drugs in blood.

An Accelerated Solvent Extraction-Solid Phase Extraction-Gas Chromatography/Mass Spectrometry Method for Determination of 18 Pesticides in Paddy

ZHANG Xiao-ting, PAN Jian-jun, ZHONG Yun, ZHUANG Yi-fei, FENG Qing-qing, YE Shu-juan

2018, 24(1): 39-46. doi: 10.16495/j.1006-3757.2018.01.007

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A gas chromatography/mass spectrometry(GC/MS) method was established for the determination of 18 pesticides in paddy based on the accelerated solvent extraction (ASE) method:in the 30 mL extraction pool under a pressure of 10.34 MPa, heating for 5 min at 80℃, and static extracting with acetonitrile for 3 min, cycling for 2 times, then washing the extraction pool with acetonitrile of 60% of the pool volume, then purging for 100 s with nitrogen. And then a solid phase extraction (SPE) column with an extraction rate of 1 drop/second was used for the purification of sample. In this method, the samples were first extracted with acetonitrile, and then purified by SPE column and evaporated to dryness in a rotary evaporator. The pretreated samples were re-dissolved in n-hexane to a constant volume for the determination by GC/MS. Linear relationships between values of peak area and mass concentration of 18 pesticides were found in the range of 0.05~1.0 μg/mL, all of their linear correlation coefficients were more than 0.99. The limits of detection were 0.104~0.647 mg/kg, and the minimum quantitative limits were 0.276~1.724 mg/kg. The spiked recoveries were between 82.5%~105.1%, and the RSDs were between 1.5%~6.4%. The method is suitable for the determination of 18 pesticides in paddy.

Determination of 5 Elements in In₂O₃-SnO₂ Sintered Mix Powder by Inductively Coupled Plasma Atomic Emission Spectrometry with Alkali-Melt

WANG Qiao, WANG Zhi-ping, SUN Hong-tao

2018, 24(1): 47-51. doi: 10.16495/j.1006-3757.2018.01.008

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A method for the determination of Fe, Ca, Mg, Al, Si in In₂O₃-SnO₂ sintered mix powder with alkali-melt, using hydrochloric acid acidification after immersed in hot water, by inductively coupled plasma atomic emission spectrometry (ICP-AES) is developed. The results showed that after the addition 0.80 g of sodium hydroxide, 0.500 0 g of the sample and fused for 120 min in an ashing furnace, the sample can be completely dissolved. The effects of matrix indium and tin can be eliminated by the matrix matching method, and no spectral interferences between the measured elements took place. Sodium salt has a certain influence on the determination of silicon, which can be eliminated by the addition of a certain amount of sodium hydroxide in standard solutions. Standard spiking test and precision were carried out. The relative standard deviations(RSD)were less than 5% and the recoveries were 90%~105%.

Determination of Fixed Carbon Content in Graphite by High Frequency Combustion-Infrared Absorption Method

YANG Yan-ming, LI Mei-yu, ZHAO Yi-hua

2018, 24(1): 52-56. doi: 10.16495/j.1006-3757.2018.01.009

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A 0.05 g sample was burned at 520℃ for 30 min, to remove the organic carbon in graphite. Then the carbonates were removed with nitric acid(1+1) and by the addition of 3 g of the carbon and sulfur analytical special mixed flux, the fixed carbon content was measured on the high frequency infrared carbon sulfur instrument. The method is simple, rapid, accurate, and reliable. The method is in good agreement with the indirect carbon fixation and non-aqueous titration volumetric methods. National standard reference materials (GBW03118, GBW03119 and GBW03120) and graphite ore samples were used to verify the method, the accuracy ranged from -0.11% to 0.04%, the precision was 0.52%~1.81%(RSD%, n=12), these indicators were in line with the DZ/T0130-2016 《geological laboratory testing quality management specification (analysis of rock and mineral samples chemical composition)》 requirements.

Practice and Exploration of Opening and Sharing of Large Scale Instruments and Equipment in Mass Spectrometry Laboratories

SONG Ni, ZHANG Xiu-li, WANG Cong, LV Zhi-hua, REN Su-mei

2018, 24(1): 57-60. doi: 10.16495/j.1006-3757.2018.01.010

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The opening and sharing of large-scale instruments and equipment in mass spectrometry laboratories of public platform is described, including the establishment of the system of the exploration and practice of opening operation model, and the shared experience and achievements. The effectiveness and problems of opening and sharing are summarized.

Exploration of Graduate Students Participating in Laboratory Large-Scale Instrument Management

FAN Guang-hua, LIU Lian, ZHANG Yong-xiang, NING Tang-yuan

2018, 24(1): 61-63. doi: 10.16495/j.1006-3757.2018.01.011

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The necessity, the operating mechanism and the implementation process of participation of graduate students in the management of large-scale instruments are expounded, a management model of "a unified management, a person specially assigned for instrument, and the combination of use and management, and the open use" has been established. Through practice, it is proved that the implementation of this measure plays a positive role in the standardization of the management of large-scale instruments, improvs the utilization ratio of instruments and accelerates the progress of laboratory scientific research projects.

2018 No. 1

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