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色谱 2017年第10期35卷 1042-1047页

作者： CHEUK Man-Yung LO Yun-Chuen POON Wing-Tat Department of Pathology Pamela Youde Nethersole Eastern Hospital

The measurement of urine catecholamine and metanephrine concentrations is important for biochemical screening and diagnosis of *** goal of this work was to develop a simple liquid chromatography-tandem mass spectrometry(LC-MS/MS)method for determining catecholamines and metanephrines in urine to replace an existing liquid chromatographic method using electrochemical *** samples were prepared using Oasis weak-cation-exchange *** eluate was analyzed on an Agilent ZORBAX Eclipse Plus Phenyl-Hexyl column in 3 ***,noradrenaline,dopamine,metanephrine,normetanephrine,and their deuterated internal standards were monitored in positive electrospray ionization mode by multiple reaction monitoring(MRM).No evidence of ion suppression was *** assay was linear up to 5μmol/L for adrenaline,5μmol/L for noradrenaline,6.1μmol/L for dopamine,5.6μmol/L for metanephrine,and 34.6μmol/L for normetanephrine,with lower limits of quantification of 5,5,12,6 and 7nmol/L,*** intra-day and inter-day precisions for all analytes ranged from 0.59%to 4.64%and1.98%to 4.80%,*** quality assurance samples were assayed and showed excellent agreement with the target *** simple method provides an improved assay for determining urine catecholamines and metanephrines.

关键词： liquid chromatography-tandem mass spectrometry (LC-MS/MS) metanephrines catecholamines pheochromocytoma urine

Determination of thyreostats in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry

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色谱 2017年第10期35卷 1048-1054页

作者： Lech RODZIEWICZ Jolanta MASLOWIECKA Anna SADOWSKA Halina CAR Laboratory of Chemical Examination of Foodstuffs Department of Veterinary Hygiene Department of Experimental Pharmacology Medical University of Bialystok

Five thyreostats(TSs),namely tapazole,thiouracil,methylthiouracil,propylthiouracil,and phenylthiouracil,were determined in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)in positive electrospray ionization *** and clean-up were achieved using a ChemElut cartridge with tert-butyl methyl ether,without a derivatization *** was achieved on an Acquity UPLC SS T3 *** mobile phase was acetonitrile and water containing 0.2%(v/v)formic *** mass spectrometer was operated in multiple reaction monitoring *** samples were spiked with TS solution at levels corresponding to 5,10,15,and 20μg/*** accuracy(internal standard corrected)ranged from 92%to 107%,with a repeatability precision(relative standard deviation,RSD)less than 15%for all five *** RSDs within-laboratory reproducibility was less than 26%.The decision limits(CCα)and detection capabilities(CCβ)were obtained from a calibration curve and were in the ranges of 3.1-6.1μg/L and 4.0-7.4μg/L,*** CCαand CCβvalues were below the recommended concentration,which was set at 10μg/*** results show that the described method is suitable for the direct detection of TSs in bovine *** method can also be used to determine TSs in porcine urine.

关键词： ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) thyreostats (TSs) urine

Liquid chromatography-tandem Mass Spectrometry Assay to Detect Ethyl Glucuronide in Human Fingernail: Comparison to Hair and Gender Differences

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American Journal of Analytical Chemistry 2012年第1期3卷 83-91页

作者： Joseph Jones Mary Jones Charles Plate Douglas Lewis Michael Fendrich Lisa Berger Daniel Fuhrmann United States Drug Testing Laboratories Inc. Des Plaines USA. Center for Addiction and Behavioral Health Research University of Wisconsin-Milwaukee Milwaukee USA.

Over the past decade, the use of hair specimens for the long-term detection of the alcohol biomarker ethyl glucuronide has been increasing in popularity and usage. We evaluated the usefulness of fingernail clippings as a suitable alterna-tive to hair for ethyl glucuronide detection. A liquid chromatography-tandem mass spectrometry method for the detection of ethyl glucuronide in fingernail clippings was fully validated and used to analyze the hair and/or fingernail specimens of 606 college-aged study participants. The limit of detection was 2 pg/mg, the limit of quantitation was 8 pg/mg and the method was linear from 8 to 2000 pg/mg. Intra- and inter-assay imprecision studies at three different concentrations (20, 40, 200 pg/mg) were all within 7.8% and all intra- and inter-assay bias studies at these levels were within 115.1% of target concentration. Ethyl glucuronide levels in fingernail (mean = 29.1 ± 55.6 pg/mg) were higher than ethyl glucuronide levels in hair (mean = 9.48 ± 22.3 pg/mg) and a correlation of the matched pairs was observed (r = 0.552, P < 0.01, n = 529). Evaluating each gender separately revealed that the correlation of male fingernail to male hair was large and significant (r = 0.782, P < 0.01, n = 195) while female hair to female fingernail was small yet sig-nificant (r = 0.249, P < 0.01, n = 334). The study results demonstrated that fingernail may be a suitable alternative to hair for ethyl glucuronide detection and may be the preferred sample type due to the lack of a gender bias.

关键词： Alcohol Biomarkers Liquid chromatography-tandem mass Spectrometry LC-MS/MS Ethyl Glucuronide Fingernail Hair

Rapid Determination of Three Kinds of Microcystins in Environmental Water Samples by Disk SPE-Ultra Performance Liquid chromatography-tandem Mass Spectrometry

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Meteorological and Environmental Research 2016年第5期7卷 62-64,68页

作者： Zhao Bin Zhang Min Zhang Fuhai Anhui Provincial Environmental Monitoring Center Station Hefei 230071 China

A method of rapidly detecting three kinds of microcystins( MCs) in environmental water samples by using disk SPE- ultra high performance liquid chromatography- tandem mass spectrometry( UPLC- MS / MS) was established. Firstly,environmental water samples were extracted by disk SPE column( C_(18)),and three kinds of MCs were separated by Waters BEH C_(18) chromatographic column with acetonitrile- 0. 2% formic acid solution as the mobile phase. After the gradient elution separation,the external standard method was used for quantitative and qualitative analysis under MRM of UPLC- MS / MS. The results showed that the three kinds of MCs in the range of 0. 05- 10 μg / L showed good linear relation,and the correlation coefficients were higher than 0. 999 4,while the method detection limit was 0. 04 ng / L. Under 0. 1,1,and 5 μg / L standard addition for the same environmental sample,the average recovery was 82. 8%- 108. 8%,and the relative standard deviation of determination results was2. 1%- 10. 1%( n = 6). This method is rapid,sensitive and accurate,so it can be effectively applied in the monitoring of MCs in environmental water samples.

关键词： Disk solid-phase extraction column Ultra performance liquid chromatography-tandem mass spectrometry Environmental water sample Microcystins Lake Chao China

Determination of okadaic acid related toxins from shellfish (<i>sinonovacula constricta</i>) by high performance liquid chromatography tandem mass spectrometry

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Agricultural Sciences 2013年第5期4卷 1-6页

作者： Hai-qi Zhang Weicheng Liu Xin He Li-jun Liang Wenyong Ding Zhong-yang He 1Zhejiang Fisheries Quality Testing Centre Hangzhou China 2College of life science Zhejiang University Hangzhou China College of Food Science and Biotechnology Engineering Zhejiang Gongshang University Hangzhou China Zhejiang Fisheries Quality Testing Centre Hangzhou China Zhejiang Mariculture Research Institute Wenzhou China

Consumption of shellfish contaminated with algal toxins produced by marine dinoflagellates can lead to diarrhetic shellfish poisoning (DSP). It was therefore essential that there are analytical techniques to identify and quantify DSP toxins in shellfish. This new methodology could facilitate DSP monitoring and create a means of rapidly responding to incidents threatening public health. In the last years there were different analytical methods for DSP, such as mouse bioassay and LC-FLD. With the development of instrument, Liquid chromatography-mass spectrometry was substituted for other analytical methods with its good sensitivity and selectivity and without derivatization for the determination of DSP. In this report, a high performance liquid chromatogra-phytandem mass spectrometric(HPLC-MS/MS)method was developed for the simultaneous determination of okadaic acid (OA) and dinophysistoxins(DTX1) in Sinonovacula constricta. Optimization of pretreatment experiment was carried out to maximize recoveries and the effectiveness. The analytes were determined under multi-reactions monitoring (MRM) scan type with tandem mass analyzer using negative ion electrospray ionization (-ESI) mode .Finally, the detection and identification of OA and DTX-1 were based upon their retention times (RT) and the fragmentation patterns of their mass spectra. The method of LOQ for the two poisons was 0.02 mg·*** real sample test showed that this method could be used for sensitive, fast, and accurate determination of the two diarrheic shellfish poisons in shellfish.

关键词： Sinonovacula Constricta High Performance Liquid chromatography-tandem Mass Spectrometry Okadaic Acid Dinophysistoxins-1

加速溶剂萃取-液相色谱-串联质谱法分析烟叶中的92种农药残留

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烟草科技 2014年第4期47卷 79-87页

作者：艾丹胡斌潘立宁陈黎刘惠民中国烟草总公司郑州烟草研究院

建立了一种同时检测烟叶中92种农药残留的加速溶剂萃取-液相色谱-串联质谱方法.通过在加速溶剂萃取池底部放置净化剂,将烟叶样品的提取、净化一步完成,之后采用液相色谱-串联质谱（LC-MS/MS）的多反应监测模式（MRM）进行分析.结果表明... 详细信息

建立了一种同时检测烟叶中92种农药残留的加速溶剂萃取-液相色谱-串联质谱方法.通过在加速溶剂萃取池底部放置净化剂,将烟叶样品的提取、净化一步完成,之后采用液相色谱-串联质谱（LC-MS/MS）的多反应监测模式（MRM）进行分析.结果表明：①最优实验条件为：提取溶剂乙腈,净化剂4 9弗罗里硅土（florisil）和40 mg石墨化炭黑（GCB）,提取温度120 ℃,提取压力10 MPa（1500 psi）,静态提取时间6 min,冲洗体积50％,静态循环2次.②目标物基质匹配标准曲线线性良好（r2＞0.99）,0.1,0.5和1 mg/kg 3种加标水平的回收率在70％～124％之间,相对标准偏差（RSD）不大于20％.该方法准确度和精密度好,适合用于烟草样品中92种农药残留的检测.

关键词：加速溶剂萃取液相色谱-串联质谱多农药残留烟草 Accelerated solvent extraction (ASE) Liquid chromatography-tandem mass spectrometry (LC-MS MS)

固相萃取-超快速液相色谱-串联质谱法同时测定血液中的4种苏丹染料

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色谱 2014年第3期32卷 224-229页

作者：朱浩黄坤玉付建飞胡岳黄娴妮陈晓红邹宝波金米聪宁波大学医学院浙江宁波315211 宁波市疾病预防控制中心浙江省微量有毒化学物健康风险评估技术研究重点实验室浙江宁波315010 宁波市疾病预防控制中心宁波市毒物研究与控制重点实验室浙江宁波315010

建立了血液样品中4种苏丹染料（苏丹Ⅰ、Ⅱ、Ⅲ和Ⅳ）的固相萃取-超快速液相色谱-串联质谱（ UFLC-MS /MS）测定方法。样品经乙腈涡旋振荡提取，上清液加等体积水稀释混匀后移入 C18固相萃取小柱净化，采用 Agi-lent Eclipse Plus C18... 详细信息

建立了血液样品中4种苏丹染料（苏丹Ⅰ、Ⅱ、Ⅲ和Ⅳ）的固相萃取-超快速液相色谱-串联质谱（ UFLC-MS /MS）测定方法。样品经乙腈涡旋振荡提取，上清液加等体积水稀释混匀后移入 C18固相萃取小柱净化，采用 Agi-lent Eclipse Plus C18色谱柱（100 mm×2.1 mm，1.8μm）以0.1％（v / v）甲酸水溶液和0.1％（v / v）甲酸乙腈溶液为流动相梯度洗脱分离，电喷雾电离（ESI）正离子多反应监测模式进行定量分析。讨论了苏丹Ⅲ和苏丹Ⅳ的偶氮基团 E-Z 光学异构现象，并对影响因素进行了分析。结果4种苏丹染料在0.1～20.0μg / L 范围内线性关系良好，相关系数均大于0.999；在低、中、高3个加标水平的平均回收率为93.0％～108.2％，相对标准偏差为4.8％～9.5％；方法的检出限（LOD）为0.06μg / L，定量限（LOQ）为0.2μg / L。本方法准确、快速、灵敏，可用于血液样品中苏丹类染料的检测分析。

关键词：超快速液相色谱-串联质谱法固相萃取苏丹染料血液 ultra-fast liquid chromatography-tandem mass spectrometry(UFLC-MS MS) sol-id-phase extraction(SPE)

反相液相色谱-串联质谱法鉴定油菜蜂花粉中的蛋白质及活性肽

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色谱 2014年第3期32卷 284-289页

作者：郭静晏嘉泽郭明靳艳大连大学环境与化学工程学院辽宁大连116622 中国科学院大连化学物理研究所中国科学院分离分析化学重点实验室辽宁大连116023

基于鸟枪法蛋白质组学分析方法,使用反相液相色谱-串联质谱(RPLC-MS/MS)系统分析油菜蜂花粉蛋白质的胰蛋白酶酶解产物,结合数据库检索,共鉴定到353条肽段。鉴定到的肽段所归属的蛋白质中有239个蛋白质可检索到其分子生物学功能,主要功... 详细信息

基于鸟枪法蛋白质组学分析方法,使用反相液相色谱-串联质谱(RPLC-MS/MS)系统分析油菜蜂花粉蛋白质的胰蛋白酶酶解产物,结合数据库检索,共鉴定到353条肽段。鉴定到的肽段所归属的蛋白质中有239个蛋白质可检索到其分子生物学功能,主要功能为结合活性、酶活性、运输活性、抑制活性等。根据血管紧张素转化酶(ACE)抑制肽活性与多肽构效之间的关系,从鉴定到的肽段中筛选并适当修饰后得到5条可能具有ACE抑制活性的肽段,化学合成肽段后进行了活性验证。结果表明5条肽段均具有良好的活性,其中肽段AELDIVLALF和LAVNLIPFP表现出较高的ACE抑制活性,半数抑制浓度(IC50)分别为(10.65±0.50)μmol/L和(23.66±1.08)μmol/L。该方法速度快,成本低,大大缩短了鉴定周期,达到了高通量筛选生物活性肽的目的。

关键词：反相液相色谱-串联质谱蛋白质血管紧张素转化酶抑制肽油菜蜂花粉 reversed-phase liquid chromatography-tandem mass spectrometry ( RPLC-MS MS)

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液相色谱-串联质谱法测定水环境中的十氯酮

色谱 2014年第3期32卷 211-215页

作者：周丽董亮史双昕张利飞张秀蓝杨文龙李玲玲黄业茹国家环境分析测试中心北京100029

建立了分析测定水环境中十氯酮的液相色谱-串联质谱法。水样经液液萃取、净化后，采用 Eclipse plus C18柱（100 mm×2.1 mm，3.5μm）分离，乙腈和水为流动相进行梯度洗脱，在电喷雾负离子多反应监测模式下进行检测，同位素内标法定量... 详细信息

建立了分析测定水环境中十氯酮的液相色谱-串联质谱法。水样经液液萃取、净化后，采用 Eclipse plus C18柱（100 mm×2.1 mm，3.5μm）分离，乙腈和水为流动相进行梯度洗脱，在电喷雾负离子多反应监测模式下进行检测，同位素内标法定量。结果表明：采用液相色谱-质谱联用技术，证实了十氯酮在甲醇中以半缩醛的形式存在，而在丙酮/乙腈中以偕二醇的形式存在。由于十氯酮极性较强，在净化时难以洗脱，并且不耐酸，所以不能与其他有机氯农药一起分析。十氯酮在5～100μg / L 范围有良好的线性关系，相关系数 r2=0.999，检出限及定量限分别为0.70 ng / L 和2.8 ng / L；在5、40和100 ng / L 3个浓度添加水平的平均回收率为95.1％～98.9％，相对标准偏差为3.85％～4.72％。本方法具有良好的灵敏度、回收率和重现性，适用于水环境中十氯酮的测定。

关键词：高效液相色谱-串联质谱十氯酮水 high performance liquid chromatography-tandem mass spectrometry( HPLC-MS MS)

高效液相色谱-串联质谱法测定比格犬血浆中的莫诺苷浓度及其药代动力学

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色谱 2014年第3期32卷 290-293页

作者：熊山李敬来朱秀清王晓英吕圭源张振清浙江中医药大学浙江杭州310053 军事医学科学院毒物药物研究所北京100850

运用高效液相色谱-串联质谱联用技术，建立了简单、快速、灵敏的比格犬灌胃莫诺苷后血药浓度的检测方法。血浆样品采用蛋白质沉淀法处理，以芍药苷作为内标，色谱柱为 Inertsil ODS-SP 色谱柱（50 mm ×2.1 mm，5μm），流动相为水（含1... 详细信息

运用高效液相色谱-串联质谱联用技术，建立了简单、快速、灵敏的比格犬灌胃莫诺苷后血药浓度的检测方法。血浆样品采用蛋白质沉淀法处理，以芍药苷作为内标，色谱柱为 Inertsil ODS-SP 色谱柱（50 mm ×2.1 mm，5μm），流动相为水（含1 mmol / L 甲酸钠）-乙腈，梯度洗脱，流速0.4 mL / min。采用电喷雾离子源（ ESI），正离子多反应监测（MRM）模式。绘制血药浓度-时间曲线，并采用 DAS 2.0软件计算药代动力学参数。方法学实验结果表明内源性杂质不干扰莫诺苷和内标的测定，线性范围为2～5000μg / L（ r =0.9966），定量限为2μg / L。方法精密度、准确度、回收率和基质效应均符合生物样品测定的要求，适合比格犬血浆中莫诺苷浓度的测定，可以应用该方法进行莫诺苷的药代动力学研究。比格犬灌胃莫诺苷3个剂量（5、15、45 mg / kg）后的血药浓度-时间曲线下面积（AUC（0-∞））分别为（1631.20±238.50）、（3984.05±750.38）、（10397.64±3156.34）μg / L＆#183;h，与给药剂量之间呈现良好的线性关系。

关键词：液相色谱-串联质谱莫诺苷血浆比格犬药代动力学 liquid chromatography-tandem mass spectrometry ( LC-MS MS )