基于UHPLC-Q-TOF/MS的不同产地普洱生茶化学成分差异研究

为了更加全面地了解产地对普洱生茶品质与化学成分的影响,本研究选取来自临沧市、普洱市、西双版纳州三大产区12个茶山(自然村)的普洱生茶样品,采用超高效液相色谱-四级杆-飞行时间质谱(UHPLC-Q-TOF/MS)对不同产地普洱生茶的非挥发性代谢物表型进行了研究。结果表明:不同产地普洱生茶的化学成分在含量上具有较大差异,且具有明显的产地特征。采用主成分分析,可以对来自西双版纳自治州(包括勐腊县、勐海县、景洪市)、普洱市、临沧市3个地级行政区的普洱生茶进行有效区分,也可以对来自普洱茶产区的东南、西南、西北3个区域的普洱生茶进行有效区分。进一步鉴定了普洱生茶中79种主要成分,并对其在12个茶山(自然村)的普洱生茶中的含量分布,以及与不同产地普洱生茶滋味品质的关系进行了分析。本研究表明,基于UHPLC-Q-TOF/MS的茶叶非挥发性化学成分轮廓可以作为普洱生茶产地判别的依据。     

Analysis of Mycosporine-Like Amino Acids in Selected Algae and Cyanobacteria by Hydrophilic Interaction Liquid Chromatography and a Novel MAA from the Red Alga Catenella repens

Mycosporine-like amino acids (MAAs), a group of small secondary metabolites found in algae, cyanobacteria, lichens and fungi, have become ecologically and pharmacologically relevant because of their pronounced UV-absorbing and photo-protective potential. Their analytical characterization is generally achieved by reversed phase HPLC and the compounds are often quantified based on molar extinction coefficients. As an alternative approach, in our study a fully validated hydrophilic interaction liquid chromatography (HILIC) method is presented. It enables the precise quantification of several analytes with adequate retention times in a single run, and can be coupled directly to MS. Excellent linear correlation coefficients (R² > 0.9991) were obtained, with limit of detection (LOD) values ranging from 0.16 to 0.43 µg/mL. Furthermore, the assay was found to be accurate (recovery rates from 89.8% to 104.1%) and precise (intra-day precision: 5.6%, inter-day precision ≤6.6%). Several algae were assayed for their content of known MAAs like porphyra-334, shinorine, and palythine. Liquid chromatography-mass spectrometry (LC-MS) data indicated a novel compound in some of them, which could be isolated from the marine species Catenella repens and structurally elucidated by nuclear magnetic resonance spectroscopy (NMR) as (E)-3-hydroxy-2-((5-hydroxy-5-(hydroxymethyl)-2-methoxy-3-((2-sulfoethyl)amino)cyclohex-2-en-1-ylidene)amino) propanoic acid, a novel MAA called catenelline.     

高效液相色谱-质谱法测定猪组织中硝基咪唑类药物残留量

建立了一种高灵敏度和高选择性的检测猪组织中硝基咪唑类药物残留的高效液相色谱-大气压化学电离质谱(APCI)法,可同时进行猪组织中3种硝基咪唑类药物残留的确证分析.本方法检测猪肌肉、肝脏、肾脏和皮下组织中硝基咪唑类药物的检测限为0.5～1μg/kg;空白组织添加硝基咪唑类药物水平为0.5、1、2或4μg/kg时,测得回收率:肌肉为61.1%～85.4%,肝脏为62.3%～80.4%,肾脏为61.6%～82.0%,皮下组织为63.6%～84.1%.     

牛奶中吡利霉素残留检测高效液相色谱-串联质谱法研究

建立了牛奶中吡利霉素残留检测的高效液相色谱-串联质谱(HPLC-MS/MS)法。液相色谱条件为:色谱柱为Waters XBridge C18柱(150 mm×2.1 mm,5μm),流动相为乙腈-0.01mol/L乙酸铵溶液(30∶70,V/V),柱温为30℃,流速为0.2 mL/min,进样量为10μL。质谱条件为:电喷雾离子源(ESI ),多反应监测(MRM)方式进行采集;监测离子质荷比(m/z)为411.5>112.0,411.5>363.4。以吡利霉素的同分异构体异吡利霉素作内标,内标法定量。结果表明:吡利霉素的线性范围为20~400 ng/mL,相关系数R2=0.999 9;方法检测限为2 ng/mL,定量限为5ng/mL;从50、100和150 ng/mL三个添加浓度检测结果可以看出,方法的平均回收率为90.4%~104.3%(n=6),批内、批间RSD均小于5%。     

液相色谱-质谱联用技术在检测食品中兽药残留的应用

动物性食品安全问题现已成为一个全球性的议题。动物性食品药残超标、安全性差的问题十分突出。建立一种准确、灵敏、可靠的分析动物性食品中兽药残留的方法刻不容缓。介绍了液相色谱-质谱联用技术(LC-MS)应用于动物性食品中几种常见兽药残留的检测方法。     

蜂蜜中氯霉素残留量检测方法研究概况

综述了近几年来国内外蜂蜜中氯霉素残留检测方法.着重介绍了高效液相色谱法、毛细管电泳法、酶联免疫法、色/质联用分析法以及生物传感器法,并分别综述了各种方法的优势与不足,最后展望了蜂蜜中氯霉素残留检测的发展趋势.     

Anti-Inflammatory Potential of Monogalactosyl Diacylglycerols and a Monoacylglycerol from the Edible Brown Seaweed Fucus spiralis Linnaeus

A monoacylglycerol (1) and a 1:1 mixture of two monogalactosyl diacylglycerols (MGDGs) (2 and 3) were isolated from the brown seaweed Fucus spiralis Linnaeus. The structures were elucidated by spectroscopic means (NMR and MS) and by comparison with the literature. Compound 1 was composed of a glycerol moiety linked to oleic acid (C18:1 Ω9). Compounds 2 and 3 contained a glycerol moiety linked to a galactose unit and eicosapentaenoic acid (C20:5 Ω3) combined with octadecatetraenoic acid (C18:4 Ω3) or linolenic acid (C18:3 Ω3), respectively. The isolated compounds were tested for their cytotoxic and anti-inflammatory activity in RAW 264.7 macrophage cells. All of them inhibited NO production at non-cytotoxic concentrations. The fraction consisting of compounds 2 and 3, in a ratio of 1:1, was slightly more effective than compound 1 (IC₅₀ of 60.06 and 65.70 µg/mL, respectively). To our knowledge, this is the first report of these compounds from F. spiralis and on their anti-inflammatory capacity.     

胶体金试纸条法和液相色谱-串联质谱法检测牛奶中四环素类药物残留比较

采用胶体金试纸条与液相色谱-串联质谱（LC-MS/MS）两种方法检测牛奶中残留的四环素类药物。结果表明：胶体金试纸条的检测限为四环素40μg/L、强力霉素40μg/L、金霉素40μg/L、土霉素80μg/L;LC-MS/MS法在牛奶中四环素、强力霉素、金霉素、土霉素的检测限为50μg/L。采用两种方法对实际样品检测,检测结果一致。与液相色谱-串联质谱法相比,胶体金试纸条具有操作简便、快速、直观的特点,可作为筛选法对样品进行定性筛查,LC-MS/MS法进行阳性样品的确证和精确定量。     

Clinical pharmacology of clemastine in healthy dogs

The pharmacokinetic properties of clemastine were investigated in six healthy dogs and compared with the effect of the drug recorded as inhibition of wheal formation induced by intradermal injections of histamine. Clemastine clearance was high (median: 2.1 L h(-1) kg(-1)) and the volume of distribution large (13.4 L kg(-1)). The half-life after intravenous administration was 3.8 h and the plasma protein binding level in vitro was 98%. After oral administration, the bioavailability was only 3%. Given intravenously, clemastine (0.1 mg kg(-1)) inhibited wheal formation completely for 7 h, whereas the effect after oral administration (0.5 mg kg(-1)) was minor. The data show that most dosage regimens suggested in the literature for the oral administration of clemastine to dogs are likely to give too low a systemic exposure of the drug to allow effective therapy.     

茚虫威对映体在番茄、葡萄及水中的液相色谱-串联质谱检测方法

建立了反相条件下茚虫威在对映体水平上的液相色谱-串联质谱(LC-MS/MS)残留分析方法。采用基质匹配标准品的外标法定量,比较分析了基质分散萃取与固相萃取2种净化方法中基质效应的影响。番茄和葡萄样品均采用乙腈提取,NH2/Carb复合固相萃取小柱净化;水样直接采用C18-H固相萃取小柱富集净化。手性拆分的色谱条件为:Chiralpak AD-RH手性分离柱,以V(乙腈)∶V(水)=65∶35为流动相,柱温25 ℃,流速0.4 mL/min。结果表明:在0.005~0.5 mg/kg(水样为mg/L)添加水平范围内,茚虫威对映体在3种基质中的回收率在65.5% ~117.0%之间,相对标准偏差(RSD,n=5)为4.1% ~18.1%。对映体的检出限(LOD)为1.4~4.3 μg/kg(μg/L),定量限(LOQ)为4.7~14.2 μg/kg(μg/L)。方法操作简便,结果稳定可靠,可用于茚虫威对映体在番茄、葡萄和水样品中残留的分析。