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Analysis of Fatty Acid in biological samples Using Liquid Chromatography–Quadrupole-Orbitrap Mass Spectrometry Under Parallel Reaction Monitoring Mode

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Journal of Analysis and Testing 2024年第2期8卷 210-217页

作者： Jingxuan Yang Wenjun Guo Xiaohang Xu Liang Zhao Yajuan Xu Yang Wang School of Pharmaceutical Sciences Changchun University of Chinese MedicineChangchun130117China Key Laboratory of Medicinal Materials Jilin Academy of Chinese Medicine SciencesChangchun130021China Jilin Ginseng Academy Changchun University of Chinese MedicineChangchun130117China

Fatty acids(FAs)are an important class of functional small molecules and participate in a variety of life biological processes.This experiment proposed a liquid chromatography–quadrupole-Qrbitrap mass spectrometry(LC–Q-Orbitrap MS)method to perform FA profiling under parallel reaction monitoring(PRM)acquisition mode.The FA was derivatized by 2-dimethylaminoethylamine(DMED)to increase the ionization e fficiency and provide the characterized fragment pattern.The mass spectra obtained from full scan,multiple ion monitoring(MIM),and PRM were compared.The results showed that the protonated ion of FA+DMED–H2O was detected and the neutral loss of 45.06 Da was observed in the tandem mass spectrum.The PRM method provided the highest selectivity and sensitivity for FA detection with the help of accurate mass weight and specific neutral loss-based fragments.The method validation was performed using the FA standards and pooled quality control serum sample,which showed that the established method had good repeatability,stability,and linearity.Finally,the developed method was successfully applied to analyze the rat serum and brain tissue samples for the drug e ffi-cacy evaluation of gross saponin of Tribulus terrestris L.fruit(GSTTF)against middle cerebral artery occlusion(MCAO)-induced ischemic stroke.This method has extensive practicability and great potential in the detection of FA,especially for the analysis of samples with complex matrices.

关键词： Fatty acid Derivatization LC-Q-Orbitrap MS Parallel reaction monitoring biological sample

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A new kinetic spectrophotometric method for the determination of major metabolite of heroin in biological samples

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Chinese Chemical Letters 2012年第5期23卷 611-614页

作者： M.Reza Shishehbore Ali Sheibani Ehsan Mirparizi Department of Chemistry Yazd BranchIslamic Azad UniversityYazd 89195-155Iran

This study describes a simple,rapid and selective catalytic kinetic spectrophotometric method for the determination of 6- monoacetylmorphine（6-MAM） as major metabolite of heroin in biological samples.The method is based upon the catalytic effect of 6-MAM on the oxidation of Janus Green by bromate in acid media.The reaction was followed spectrophotometrically by measuring the decrease in absorbance of Janus Green at 618 nm.The dependence of sensitivity on the reaction variables was studied.Under optimum conditions,two linear calibration curves over the range 0.1-1.0μg mL^（-1） and 1.0-34.0μg mL^（-1） of 6- MAM were obtained.The detection limit was 1.2×10~2μg mL^（-1） of 6-MAM.The relative standard deviations for six replicate determinations of 0.8 and 5.0μg mL^（-1） of 6-MAM were 1.4 and 1.1%respectively.The effect of various species commonly associated with heroin in real samples was also investigated.The proposed method was successfully applied in human urine and serum samples with satisfactory results.

关键词： Heroin metabolite 6-Monoacetylmorphine Janus Green Kinetic spectrophotometric biological sample

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Determination of thorium in the hair and urine of workers and the public in a rare earth mining area

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Radiation Medicine and Protection 2022年第2期3卷 91-95页

作者： Yao Zhang Xianzhang Shao Xiangyin Kong Liangliang Yin Chengguo Wang Liang Lin Yanqin Ji China CDC Key Laboratory of Radiological Protection and Nuclear Emergency National Institute for Radiological ProtectionChinese Center for Disease Control and PreventionBeijing 100088China Institute for Radiological Protection Inner Mongolia Center for Disease of Control and PreventionHohhotInner Mongolia 010031China Baotou Municipal Center for Disease Control and Prevention BaotouInner Mongolia 014030China

Objective:To assess the thorium exposure of the mine workers and the public to a typical rare earth mine and estimate the resultant committed effective dose to them.Methods:A total of 79 volunteers were selected in this survey,including 69 mine workers and 10 local residents living about 4 km away from the mine site.Urinary samples were collected from 79 volunteers,with 65 hair samples from 57 workers and 8 local residents.The thorium concentrations in urinary and hair samples were determined by using inductively coupled plasma mass spectrometry.The committed effective doses were estimated based on the urinary samples collected and the parameters as recommended by ICRP Publication 137.Results:Thorium concentrations in the samples from the workers ranged from 19.0 to 2388.8 ng/g in hair with median of 149.8 ng/g,and in urine 18.3–906.1 ng/L with median of 59.6 ng/L,respectively.The median values of thorium concentrations were 11.8 ng/g in hair and 32.40 ng/L in urine for the public respectively.The thorium concentrations in urinary and hair samples of the workers were not only higher than those of the residents in the local area,but also than those of non-occupationally exposed populations as reported.The median values of committed effective dose were estimated to be 1.51 mSv for the workers and 781μSv for the local residents,respectively.Conclusions:The residents in the local area,and especially the workers,have been subject to long term thorium exposure.More attention should be paid to the radiological hazards of thorium to the workers and local residents.

关键词： biological sample Occupational exposure Radioactive contamination Committed effective dose Thorium

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Determination of Trace Rare Earth Elements in biological samples by ICP-AES with Tungsten-spiral Electrothermal Vaporization Sampling

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Journal of Rare Earths 1993年第1期11卷 52-57页

作者：梅二文刘慧廖振环江祖成 Department of chemistry wuhan UniversityWuhan 430072China Author to whom correspondence should be sent

A method for determination of trace rare earth elements in biological sample by ICP-AES with tungsten-spiral electrothermal vaporization(TETV-ICP-AES)sampling has been developed in this work. Several influencing factors including desolvation and vaporization parameters,carrier gas flow rate and ma- trix effect were investigated in detail.Under optimal experimental conditions,the detection limits for La,Nd, Gd,Dy,Ho,Yb,Lu and Y were obtained in the range of 10^(-9)～10^(-11) g,and they are comparable to and,in most instances,better than those for the GFAAS and conventional pneumatic nebulisation-ICP-AES.The precision(RSD)obtained for this method is less than 6%.

关键词： Tungsten-spiral electrothermal vaporization sampling ICP-AES REE biological sample

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NON-DESTRUCTIVE ANALYSIS OF THE NUCLEI OF TRANSGENIC LIVING CELLS USING LASER TWEEZERS AND NEAR-INFRARED RAMAN SPECTROSCOPIC TECHNIQUE

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Genomics, Proteomics & Bioinformatics 2005年第3期3卷 169-178页

作者： Wei Tang Ronald J. Newton Chang-An Xie Yong-Qing Li Nicki Whitley Department of Biology Howell Science Complex East Carolina UniversityGreenville NC 27858-4353 USA. Department of Physics Howell Science Complex East Carolina University Greenville NC 27858-4353 USA.

Transgenic cell lines of loblolly pine （Pinus taeda L.） were analyzed by a compact laser-tweezers-Raman-spectroscopy （LTRS） system in this investigation. A low power diode laser at 785 nm was used for both laser optical trapping of single transgenic cells and excitation for near-infrared Raman spectroscopy of the nuclei of synchronized cells, which were treated as single organic particles, at the S-phase of the cell cycle. Transgenic living cells with gfp and uidA genes were used as biological samples to test this LTRS technique. As expected, different Raman spectra were observed from the tested biological samples. This technique provides a high sensitivity and enables real-time spectroscopic measurements of transgenic cell lines. It could be a valuable tool for the study of the fundamental cell and molecular biological process by trapping single nucleus and by providing a wealth of molecular information about the nuclei of cells.

关键词： transgenic cell laser optical trapping near-infrared Raman spectroscopy biological sample

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Validation of an Optimized Spectrophotometric Method for the Selective Determination of Labetalol Hydrochloride

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Chinese Journal of Chemistry 2005年第12期23卷 1611-1617页

作者： RAHMAN, Nafisur SINGH, Manisha HODA, Nasrul Md ZAIDI, S.M. Kashif R. BANU, Naheed Analytical Research Laboratory Department of Chemistry Aligarh Muslim University Aligarh-202 002 India Department of Biochemistry Faculty of Life Science Aligarh Muslim Universtty Aligarh-202002 India

A simple sensitive and economical method for the determination of labetalol hydrochloride has been proposed, based on the reaction of labetalol with sodium nitroprusside and hydroxylamine hydrochloride in sodium dihydrogen phosphate-sodium hydroxide buffer solution of pH 12. The green-blue color produced due to the formation of a nitroso derivative has been measured at 695 nm. The Beer＇s range was obeyed in the concentration range of 2-51 μg·mL^-1 with molar absorptivity of 0.48 × 10^4 L·mol^-1·cm^-1. Rigorous statistical analyses were performed for the validation of the method. A detailed investigation of the selectivity of the method has been done to find it to be highly selective for the determination of labetalol hydrochloride in the presence of its acidic degradation product and common excipients of formulations. The proposed method was successfully applied to the determination of labetalol hydrochloride in the laboratory prepared dosage forms. Comparison of the means of the proposed procedure with a reference method using point as well as interval hypotheses showed no statistically significant difference. The developed method was extended to investigate its applicability to biological samples.

关键词： labetalol hydrochloride sodium nitroprusside hydroxylamine hydrochloride biological sample

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色质联用技术在毒物分析中的应用

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分析测试学报 2004年第Z1期23卷 62-63页

作者：王芳琳王北榆公安部物证鉴定中心北京100038 北京市公安局平谷分局北京100000

　　从生物样品中检测未知物,一直以来是毒物分析中的一个难点.如何有效地提取目标化合物,并选择适合的检测手段将未知物筛选出来,GC-MS方法是快速筛选多种毒物和药物的一个简便、可靠的手段.随着MS技术的不断发展,更灵敏、更准确的特... 详细信息

　　从生物样品中检测未知物,一直以来是毒物分析中的一个难点.如何有效地提取目标化合物,并选择适合的检测手段将未知物筛选出来,GC-MS方法是快速筛选多种毒物和药物的一个简便、可靠的手段.随着MS技术的不断发展,更灵敏、更准确的特性将使其成为药物和毒物分析中必不可少的一门技术.……

关键词： Poison biological sample GC-MS

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色质联用技术在毒物分析中的应用

色质联用技术在毒物分析中的应用

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2004年全国有机质谱学术交流会

作者：王芳琳王北榆公安部物证鉴定中心北京市公安局平谷分局

从生物样品中检测未知物,一直以来是毒物分析中的一个难点。如何有效地提取目标化合物, 并选择适合的检测手段将未知物筛选出来,GC-MS方法是快速筛选多种毒物和药物的一个简便、可靠的手段。随着MS技术的不断发展,更灵敏、更准确的特性... 详细信息

从生物样品中检测未知物,一直以来是毒物分析中的一个难点。如何有效地提取目标化合物, 并选择适合的检测手段将未知物筛选出来,GC-MS方法是快速筛选多种毒物和药物的一个简便、可靠的手段。随着MS技术的不断发展,更灵敏、更准确的特性将使其成为药物和毒物分析中必不可少的一门技术。1 实验部分1.1实验设备及材料气相色谱-质谱联用仪:岛津5050A,GC-MS。1.2实验方法1.2.1顶空法称取生物样品(血液、胃组织、肝脏、肺、肾脏等)2 mL(g),置顶空瓶中,密封,80

关键词： Poison biological sample GC - MS

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基于电喷雾萃取电离质谱分析的原位活体检测技术

基于电喷雾萃取电离质谱分析的原位活体检测技术

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中国有机质谱学第十四届全国学术大会

作者：陈焕文丁建华任玉林费强吉林大学化学院

质谱法具有高灵敏度,高特异性和适用范围广等特点。很多年前,人们就对未来小型质谱仪在诊所和太空中的应用做了科学预测。然而,由于传统的质谱分析需要复杂的样品预处理过程,究竟如何才能够方便快捷而且科学地将质谱仪应用到疾病诊断中... 详细信息

质谱法具有高灵敏度,高特异性和适用范围广等特点。很多年前,人们就对未来小型质谱仪在诊所和太空中的应用做了科学预测。然而,由于传统的质谱分析需要复杂的样品预处理过程,究竟如何才能够方便快捷而且科学地将质谱仪应用到疾病诊断中呢,直到电喷雾萃取电离(EESI)技

关键词： EESI in vivo analysis biological sample clinic diagnosis explosives

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