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Speciation Analysis of Arsenic Compounds in Seafood by Ion chromatography-Atomic Fluorescence Spectrometry

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New antimyeloma drugs in spinal cord infiltration for multiple myeloma. Determination of lenalidomide incerebrospinal fluid with ultrasensitive high-performance liquid chromatography

中国海洋大学学报（英文版） 2017年第3期 455-460页

作者： HAN Tingting JI Hongwei LI Huixin CUI He Song Tian DUAN Xiaojuan ZHU Qianlin CAI Feng ZHANG Li College of Chemistry and Chemical Engineering，Ocean University of China Shandong Entry-Exit Inspection and Quarantine Technology Center School of Science，Yanshan University Qingdao Entry-Exit Inspection and Quarantine Bureau

Ion chromatography-ultra violet-hydride generation-Atomic Florescence Spectrometry was applied to detect 5 arsenic species in seafoods. The arsenic species studied include arsenobetaine（As B）, arsenite（As（III））, dimethylarsinic acid（DMA）, monomethylarsonic acid（MMA）, and arsenate（As（V））, which were extracted from samples using 2% formic acid. Gradient elution using 33 mmol L-1 CH3COONH4 and 15 mmol L-1 Na2CO3 with 10 mL CH3CH2OH at pH 8.4 allowed the chromatographic separation of all the species on a Hamilton PRP-X100 anion-exchange column in less than 8 min. In this study, an ultrasound extraction method was used to extract arsenic species from seafood. The extraction efficiency was good and the recoveries from spiked samples were in the range of 72.6%–109%; the precision between sample replicates was higher than 3.6% for all determinations. The detection limits were 3.543 μg L-1 for As B, 0.4261 μg L-1 for As（III）, 0.216 μg L-1 for DMA, 0.211 μg L-1 for MMA, and 0.709 μg L-1 for As（V）, and the linear coefficients were greater than 0.999. We also developed an application of this method for the determination of arsenic species in bonito, Euphausia superba, and Enteromorpha with satisfactory results. Therefore, it was confirmed that this method was appropriate for the detection of arsenic species in seafood.

关键词： arsenic species seafood ion chromatography atomic fluorescence spectrometry

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TLC Identification and Extraction Process of Rubiasin-1-methyl Ether from Yao Medicine Chuanlianzhu

Modern Chemotherapy（化疗） 2012年第2期 11-13页

作者： Inmaculada Rapado Juan José Lahuerta Laura Montejano María Ángeles Montalbán Laura Pares Joaquín Martínez- López

A 64-year-old woman with IgA kappa multiple myeloma was treated with thalidomide-dexa- methasone. Due to progression of the disease, bortezomib, doxorubicin and dexamethasone were administered, followed by autologous stem cell transplantation. Although near-complete remission was achieved, 5 months later, neuro- logical symptoms appeared and the patient was diagnosed with multiple myeloma with cells in- filtrating the spinal cord. Bis-chloronitrosourea, bortezomib and lenalidomide were then admin- istered and although the patient remained neu- rologically asymptomatic, she died 3 months later becausee of disease progression. Lena- lidomide entered into the cerebrospinal fluid (confirmed by ultrasensitive high-performance liquid chromatography), although did not im- prove the poor prognosis of multiple myeloma involving the central nervous system.

关键词： Lenalidomide Multiple Myeloma Spinal Cord Infiltration High-Performance Liquid chromatography

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Medicinal Plant 2024年第3期15卷 35-38页

作者： Jingrong LU Jiangcun WEI Xiumei MA Bing QING Meiyan QIU Wen ZHONG Guangxi International Zhuang Medicine Hospital Nanning 530201China

[Objectives]To establish a thin-layer chromatography(TLC)method for the determination of rubiadin-1-methyl ether in Yao Medicine Chuanlianzhu(Damnacanthus giganteus).[Methods]A silica gel G thin-layer plate was adopted for *** ether(60-90℃)-chloroform-methanol-water(7:15:3:1)was used as the developing solvent and inspected under ultraviolet lamp(365 nm).The content was determined by Inertsil ODS-3 C 18 column(4.60 mm×250 mm,5μm),mobile phase:acetonitrile-0.2%phosphoric acid gradient elution,detection wavelength 277 nm,flow rate 1.0 mL/min,column temperature 30℃,injection volume 10μL.[Results]The spots of 10 Chuanlianzhu samples from different origins showed the same color at the same position as the control,and the spots were clear and *** injection volume of rubiadin-1-methyl ether showed a good linear relationship in the range of 2.90-145μg(R=0.9996).The average recovery rate of rubiadin-1-methyl ether in the low,medium and high dose groups of Yao Medicine Chuanlianzhu was 98.72%,and RSD=1.78%.[Conclusions]This method can effectively identify Yao Medicine Chuanlianzhu medicinal materials and accurately determine the content of rubiadin-1-methyl ether in the medicinal *** provides a scientific basis for the development and utilization of Yao Medicine Chuanlianzhu medicinal resources.

关键词： Chuanlianzhu Thin-layer chromatography (TLC) Extraction process Rubiadin-1-methyl ether Content determination

分散液液微萃取-反相液液微萃取-扫集-胶束电动色谱法测定红酒中的3种氯酚类物质

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色谱 2014年第3期32卷 256-262页

作者：孙建芝贺晖刘书慧西北农林科技大学理学院陕西杨凌712100 旱区作物逆境生物学国家重点实验室陕西杨凌712100

建立了分散液液微萃取（DLLME）-反相液液微萃取（RP-LLME）-扫集-胶束电动色谱富集模型，并用于红酒中五氯酚（PCP）、2，4，6-三氯酚（TCP）和2，4-二氯酚（DCP）3种氯酚的测定。实验考察了两步微萃取的萃取参数对氯酚萃取率的影响和... 详细信息

建立了分散液液微萃取（DLLME）-反相液液微萃取（RP-LLME）-扫集-胶束电动色谱富集模型，并用于红酒中五氯酚（PCP）、2，4，6-三氯酚（TCP）和2，4-二氯酚（DCP）3种氯酚的测定。实验考察了两步微萃取的萃取参数对氯酚萃取率的影响和样品分离富集的电泳条件。最佳萃取条件 DLLME 为：3.5 mL 红酒（ pH 3.0，120 g / L NaCl），300μL 正己烷（萃取剂）；RP-LLME 为：25μL 0.16 mol / L NaOH（萃取剂）。最佳电泳条件：25 mmol / L NaH2 PO4，100 mmol / L 十二烷基硫酸钠（ SDS），30％（ v / v）乙腈，pH 2.3；分离电压-15 kV；样品基质为80 mmol / L NaH2 PO4；压力进样20 s×20.67 kPa（3 psi）。PCP 和 TCP 的线性范围为0.5～100μg / L（ r≥0.9910）， DCP 的线性范围为1.5～80μg / L（r =0.9851）。3种分析物的检出限（ S / N =3）为0.035～0.114μg / L，加标回收率为75.2％～104.7％，相对标准偏差≤6.17％。该方法富集倍数高、灵敏度高、重现性好、分析速度快，可为不同样品基质中痕量氯酚污染物及某些弱酸性有机污染物测定提供参考。

关键词：分散液液微萃取反相液液微萃取扫集胶束电动色谱氯酚红酒 dispersive liquid-liquid microextraction( DLLME ) reversed phase liquid-liquid microextraction( RP-LLME ) micellar electrokinetic chromatography ( MEKC ) chlorophenols(CPs)

新型吡咯烷键合反相高效液相色谱固定相的制备与研究（英文）

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色谱 2017年第11期35卷 1120-1128页

作者： Elahe NAGHDI Kourosh TABAR HEYDAR Ali SHARIFI Seyyed Hamid AHMADI Chemistry and Chemical Engineering Research Center of Iran

A new ionic liquid-based high-performance liquid chromatography stationary phase is reported.A derivative of N-methyl pyrrolidinium tetrafluoroborate was covalently immobilized on the surface of silica particles to prepare silica-based N-methyl pyrrolidinium tetrafluoroborate(SilprMP BF4)stationary *** obtained ionic liquid-modified silica was evaluated and confirmed by elemental analysis,infrared spectroscopy,and thermogravimetric analysis.A column was packed with the modified *** retention behavior of aromatic compounds,alkyl benzenes,and acidic and basic compounds on the SilprMP BF4 stationary phase was studied under reversed-phase liquid chromatography *** effect of the eluent pH on the separation of the acidic and basic compounds was also *** new stationary phase involves multiple retention mechanisms,such as electrostatic,hydrophobic,ion-dipole,and anion-exchange interactions,which might lead to multipurpose separation media.

关键词： reversed-phase high-performance liquid chromatography stationary phase ionic liquids (ILs) pyrrolidinium

超高效液相色谱-线性离子阱/静电场轨道阱高分辨质谱快速筛查化妆品中的24种激素

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色谱 2014年第5期32卷 477-484页

作者：李兆永王凤美牛增元罗忻张罡陈军辉国家海洋局第一海洋研究所海洋生态研究中心山东青岛266061 山东出入境检验检疫局检验检疫技术中心山东青岛266002

建立了超高效液相色谱-线性离子阱/静电场轨道阱组合式高分辨质谱联用(UPLC-LTQ/Orbitrap MS)快速筛查、定性识别化妆品中24种激素的分析方法。不同剂型的化妆品样品经甲醇超声提取,用Waters ACQUITY UPLC BEH C18色谱柱(50 mm×2.1 mm,... 详细信息

建立了超高效液相色谱-线性离子阱/静电场轨道阱组合式高分辨质谱联用(UPLC-LTQ/Orbitrap MS)快速筛查、定性识别化妆品中24种激素的分析方法。不同剂型的化妆品样品经甲醇超声提取,用Waters ACQUITY UPLC BEH C18色谱柱(50 mm×2.1 mm,1.7μm)分离,以乙腈和0.1%(v/v)甲酸水溶液为流动相进行梯度洗脱。通过静电场轨道阱全扫描得到激素化合物的准分子离子的精确质量数,实现对化妆品中激素的快速筛查;再以保留时间和数据依赖扫描(data dependent scan)模式获得的子离子质谱图进行定性确证。24种激素化合物的质量准确度误差小于3×10-6(3 ppm);线性良好,相关系数大于0.99;检出限≤10μg/kg(S/N=3),能满足实际化妆品样品的分析要求。应用该方法对不同剂型的50余种化妆品样品进行筛查分析,结果良好。该方法是化妆品中激素快速筛查、定性识别的有效方法。

关键词：超高效液相色谱线性离子阱静电场轨道阱组合质谱激素化妆品 ultra high performance liquid chromatography ( UPLC ) linear ion trap orbitrap mass spectrometry( LTQ Orbitrap MS)

凝胶渗透色谱-高效液相色谱-线性离子阱质谱法测定膳食样品中的氨基甲酸酯类农药残留

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色谱 2014年第5期32卷 499-505页

作者：杨欣李鹏苗虹赵云峰吴永宁国家食品安全风险评估中心北京100021 卫生部食品安全风险评估重点实验室北京100021

建立了高效液相色谱-线性离子阱质谱（ HPLC-LIT-MS）测定膳食样品中氨基甲酸酯类农药的检测方法。样品中加入同位素内标，用正己烷饱和的乙腈超声提取，凝胶渗透色谱净化。以乙腈和含5 mmol/L 甲酸铵和0.1％（v/v）甲酸的水溶液为流动... 详细信息

建立了高效液相色谱-线性离子阱质谱（ HPLC-LIT-MS）测定膳食样品中氨基甲酸酯类农药的检测方法。样品中加入同位素内标，用正己烷饱和的乙腈超声提取，凝胶渗透色谱净化。以乙腈和含5 mmol/L 甲酸铵和0.1％（v/v）甲酸的水溶液为流动相，目标化合物经 CAPCELL PAK CR（100 mm＆#215;2.1 mm，5μm；SCX-C18（1：4））色谱柱分离，梯度洗脱，流速0.2 mL/min。采用电喷雾电离，选择反应监测（ SRM）正离子模式三级离子监测。内标法定量。膳食类样品中氨基甲酸酯农药的平均加标回收率在60.4％~114％之间；相对标准偏差在3.46％~16.2％范围内；检出限（ LODs）在0.001~0.010 mg/kg之间。应用所建立的方法对2007年第四次中国总膳食研究项目的9类膳食样品基质中的氨基甲酸酯类农药进行了检测，在少量样品中检出了涕灭威和克百威。

关键词：凝胶渗透色谱高效液相色谱-线性离子阱质谱氨基甲酸酯类农药膳食 gel permeation chromatography( GPC) high performance liquid chromatography ( HPLC) linear ion trap mass spectrometry( LIT-MS)

柱前衍生高效液相色谱法同时测定水性涂料中6种醛类化合物

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色谱 2014年第3期32卷 230-234页

作者：陈潜周宇艳程欲晓林苗东华大学化学化工与生物工程学院生态纺织教育部重点实验室上海201620 上海出入境检验检疫局工业品与原材料检测技术中心上海200135

建立了柱前衍生高效液相色谱同时测定水性涂料中甲醛、乙醛、丙醛、苯甲醛、正戊醛和对甲基苯甲醛等6种醛类化合物的方法。样品经水超声提取后，与2，4-二硝基苯肼乙腈溶液在酸性条件下衍生，再经0.45μm 针式过滤器过滤后进样分析。系... 详细信息

建立了柱前衍生高效液相色谱同时测定水性涂料中甲醛、乙醛、丙醛、苯甲醛、正戊醛和对甲基苯甲醛等6种醛类化合物的方法。样品经水超声提取后，与2，4-二硝基苯肼乙腈溶液在酸性条件下衍生，再经0.45μm 针式过滤器过滤后进样分析。系统考察了酸度调节剂、pH 值、反应温度、时间等因素对衍生反应的影响，优化的反应条件为：以稀释后的盐酸溶液作为酸度调节剂，缓冲溶液 pH =3，反应温度为60℃，反应时间为30 min。在此条件下，于0.08～2.0 mg / L 浓度范围内，6种醛类化合物呈良好的线性关系；检出限为0.05～2.50 mg / kg；在2.0、4.0、6.0 mg / kg 3个水平下的加标回收率为87.0％～112.8％；RSD 为1.12％～9.54％。结果表明，本方法具有较宽的线性范围，良好的精密度和准确度，适用于水性涂料中6种醛类化合物的同时测定。

关键词：柱前衍生高效液相色谱法醛类化合物 2,4-二硝基苯肼水性涂料 high performance liquid chromatography ( HPLC )

抑制型电导检测离子交换色谱法测定1,4-丁烷二磺酸盐

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色谱 2006年第5期24卷 535-536页

作者：樊慧丁明玉清华大学化学系有机磷与化学生物学教育部重点实验室北京100084

腺苷蛋氨酸，简称：SAMe，商吕是存在于各种生物体内的一种天然物质，它主要作为甲基供体参与各种栈促转甲基过程，并通过转巯基作为合成牛磺酸、半胱氨酸及谷胱甘肽的前体。

关键词：离子交换色谱法(ion exchange chromatography IEC) 抑制型电导检测(suppressed conductivity detection) 1 4-丁烷二磺酸盐(1 4-butanedisulphonate) 思美泰(Transmetil) 腺苷蛋氨酸(S—adenosyl-L-metionine)