基于UPLC-Q-TOF-MS/MS的沉香2-(2-苯乙基)色酮聚合物成分分析

为了明确沉香（Aquilaria spp.）药材中2-(2-苯乙基)色酮聚合物（PPECs）组分及其结构,本研究采用超高效液相色谱-串联四级杆-飞行时间质谱法（UPLC-Q-TOF-MS/MS）采集沉香样品一级与二级质谱图,对PPECs的质谱裂解途径进行分析,对沉香药材中PPECs组分进行筛查与结构确证。共鉴定出PPECs组分55个,根据结构特征,55个组分分属于3种结构类型,即2-(2-苯乙基)色酮二聚物（DPECs）、2-(2-苯乙基)色酮三聚物（TPECs）和萜类-2-(2-苯乙基)色酮二聚物（SPECs）。鉴定的全部组分包括44个DPECs、3个TPECs和8个SPECs,其中9个DPECs、1个TPECs和1个SPECs首次在沉香中被发现;其次,沉香PPECs的部分组分具有2～4个同分异构体。综上,沉香药材中PPECs组分及其同分异构体丰富,且DPECs类型的组分在总PPECs中所占比例最高（80%）。该研究结果可为沉香药效物质基础研究及开发利用提供参考。     

利用超高效液相色谱-飞行时间-串联质谱法分析青刺果油中的脂质成分

青刺果为多年生稀有木本油料植物,是我国特有民族野生资源。在对青刺果油中脂肪酸组成分析的基础上,建立了超高效液相色谱-飞行时间-串联质谱的脂质分析方法,对其所含脂质的种类、组成、相对含量作分析。 结果显示,在青刺果油主要脂肪酸的含量为：油酸39.17%、亚油酸36.16%、棕榈酸16.38%;从比例上看,饱和脂肪酸: 单不饱和脂肪酸:多不饱和脂肪酸比例接近0.6:1:1。共鉴定出169种脂质,包括76种磷脂,84种甘油酯和9种糖脂; 其中磷脂、甘油酯和糖脂的主要成分分别为磷脂酰肌醇、甘油三酯和双半乳糖甘油二酯。     

番橄榄脂溶性成分比较分析

用正己烷提取番橄榄干燥果实的脂溶性成分,经GC-MS分析,共鉴定出26个成分,其中青果中主要成分有烷烃类(34.58%),甾体化合物类(30.25%),醇类(10.04%),酯类(6.02%);黄熟果中主要成分有烷烃类(47.23%),醇类(15.72%),甾体化合物类(12.08%),酯类(6.76%)。用UPLC-MS/MS对其中的β-谷甾醇和维生素E进行了定性定量测定,结果表明:番橄榄青果中β-谷甾醇的含量为2286.5 mg/kg,维生素E的含量为5.0 mg/kg;黄熟果中β-谷甾醇的含量为925.5 mg/kg,维生素E的含量为52.0 mg/kg。通过与已报道的关于番橄榄成分的文章比较,并分析结果差异产生的原因。     

基于UPLC-MS/MS技术的代谢组学方法研究铝胁迫下花生的根系代谢

为有效降低铝毒害,探讨铝胁迫下花生幼苗根系代谢变化,以花育23（H,铝敏感型）和粤油7号（Y,耐铝型）两个花生品种为材料,基于超高效液相色谱-串联质谱法（UPLC-MS/MS）的广泛靶向代谢组学,研究铝胁迫对花生根系的影响。结果发现,从两个花生品种的幼苗根系中检测出416种代谢产物,与对照（HC）相比,花育23（HA）共筛选出155个差异代谢物（即HC vs HA）,其中上调代谢物为27种,下调为128种;粤油7号（即YC vs YA）共筛选出109个差异代谢物,其中上调代谢物为28种,下调为81种。铝胁迫下两个花生品种幼苗根系之间（即HA与YA之间）筛选出145个差异代谢物,其中上调代谢物为76种,下调为69种。代谢物主要集中在酚酸类、黄酮、有机酸、木脂素和香豆素、氨基酸及其衍生物和核苷酸及其衍生物等。KEGG代谢通路富集分析显示,这些差异代谢物主要富集在异黄酮生物合成代谢通路上。铝胁迫下,花生幼苗根系代谢物发生的明显改变,可为花生生产有效降低铝毒害提供依据。     

猴耳环多酚的大孔树脂纯化工艺及其组分分析

建立并优化猴耳环多酚的纯化工艺并对其组分进行定性分析.本研究以猴耳环多酚粗提物为原料,以吸附及解吸附效果筛选了最优大孔树脂,再以吸附、解吸附和纯度为评价指标,考察各工艺参数对AB-8树脂纯化多酚的影响,最后采用超高效液相色谱-四级杆-飞行时间串联质谱(UPLC-Q-TOF-MS)法进行多酚组成定性分析.结果表明:优选A...     

UPLC-MS/MS法测定水稻中噁唑酰草胺和氰氟草酯及其代谢物的残留及膳食风险评估

建立了使用分散固相萃取的QuEChERS前处理方法,并通过超高效液相色谱串联质谱(Ultra Performance Liquid Chromatography Tandem Mass Spectrometry,UPLC-MS/MS)对糙米、稻壳和秸秆样品中的噁唑酰草胺和氰氟草酯及其代谢物成功进行了定量测定.结果 表明...     

基于液相色谱-串联质谱法分析不同植物油经加热处理前后氧化脂肪酸的变化

植物油中的氧化脂肪酸主要是亚油酸(linoleic acid, LA)和亚麻酸(linolenic acid, ALA)等多不饱和脂肪酸在酶、光照、加热等条件下产生的过氧化羟基脂肪酸(hydroperoxyl fatty acid)、羟基脂肪酸(hydroxy fatty acids)和环氧基脂肪酸(epoxy fatty acid)等。这些氧化脂肪酸的变化在一定程度上反映了油脂本身的氧化稳定性和氧化初期的变化,可作为植物油氧化初级阶段标志物。本研究基于高效液相色谱-三重四极杆质谱(high performance liquid chromatography triple quadrupole mass spectrometry,HPLC-Qq Q-MS/MS)联用技术,对室温和180℃加热处理30min后的菜籽油、葵花油、紫苏油、亚麻籽油中氧化脂肪酸进行了定性和定量分析。结果表明,相比于室温,经180℃加热处理30min,4种植物油中的LA、ALA等多不饱和脂肪酸含量下降;大部分LA、ALA类氧化脂肪酸的含量明显提高。经主成分分析(Principal component analysis, PCA),不同种类和处理下的植物油样本聚类明显,差异显著;经偏最小二乘法判别分析(Partial least squares discriminant analysis,PLS-DA),发现了植物油加热氧化初期的13-HODE、13-oxo-ODE、12,13-Ep OME、9,10-Ep ODE、12,13-Ep ODE、15,16-Ep ODE六种潜在的标志物,本研究对植物油氧化初期的评价以及植物油氧化初级阶段机制的深入研究具有一定的指导意义。     

基于壳聚糖/氧化石墨烯/硅藻土固相萃取-液相色谱串联质谱测定茶叶中多种农药残留

利用前期合成的壳聚糖/氧化石墨烯/硅藻土固相萃取柱高效吸附茶叶基质,结合超高效液相色谱串联质谱（UPLC-MS/MS）,建立了茶叶中46种农药残留的分析方法。茶叶样品经乙腈提取,固相萃取柱净化,乙腈淋洗等样品前处理,UPLC-MS/MS分析46种农药残留。结果表明,该新型固相萃取净化柱可以高效吸附去除茶叶基质,大大降低基质效应,绿茶、红茶和乌龙茶中农药的基质效应分别下降了4.7%~66.5%,3.2%~35.5%和4.4%~42.8%。在3个加标水平下,46种农药回收率在61.5%~118%线性良好,相关系数（R²）均大于0.98。所建立方法具有吸附剂用量少、省时、无需基质标准溶液、可以检测不同茶类多农残和定量限低等优点。     

Accurate Dereplication of Bioactive Secondary Metabolites from Marine-Derived Fungi by UHPLC-DAD-QTOFMS and a MS/HRMS Library

In drug discovery, reliable and fast dereplication of known compounds is essential for identification of novel bioactive compounds. Here, we show an integrated approach using ultra-high performance liquid chromatography-diode array detection-quadrupole time of flight mass spectrometry (UHPLC-DAD-QTOFMS) providing both accurate mass full-scan mass spectrometry (MS) and tandem high resolution MS (MS/HRMS) data. The methodology was demonstrated on compounds from bioactive marine-derived strains of Aspergillus, Penicillium, and Emericellopsis, including small polyketides, non-ribosomal peptides, terpenes, and meroterpenoids. The MS/HRMS data were then searched against an in-house MS/HRMS library of ~1300 compounds for unambiguous identification. The full scan MS data was used for dereplication of compounds not in the MS/HRMS library, combined with ultraviolet/visual (UV/Vis) and MS/HRMS data for faster exclusion of database search results. This led to the identification of four novel isomers of the known anticancer compound, asperphenamate. Except for very low intensity peaks, no false negatives were found using the MS/HRMS approach, which proved to be robust against poor data quality caused by system overload or loss of lock-mass. Only for small polyketides, like patulin, were both retention time and UV/Vis spectra necessary for unambiguous identification. For the ophiobolin family with many structurally similar analogues partly co-eluting, the peaks could be assigned correctly by combining MS/HRMS data and m/z of the [M + Na]⁺ ions.     

固相萃取-GC/LC-MS/MS测定茶叶中79种农药残留

建立了一套以一次固相萃取前处理方法,运用气相色谱-串联质谱（GC-MS/MS）和液相色谱-串联质谱（LC-MS/MS）两种检测技术,测定茶叶中79种农药残留的可靠、快速、高通量检测方法。该方法用20βmL乙腈一次均质提取,分取提取液10βmL,用乙腈+甲苯（3∶1）20βmL洗脱过Carbon/NH₂小柱净化,用5βmL乙腈定容混匀,于GC-MS/MS和LC-MS/MS同时检测。结果表明,79种农药在0.01~0.40βmg·L^-1范围内线性良好,相关系数（R²）在0.995以上;高、低、中3种水平加标回收率在67.3%~130.8%内;相对标准偏差（RSD）在15%内;98.7%的农药定量限（LOQ）≤0.01βmg·kg^-1;使用多种类茶叶实际检测,结果均合格。因此,该方法能同时检测含有机磷、有机氯、拟除虫菊酯类、氨基甲酸酯类和有机杂环类5大类农药,更有利于大批量茶叶样品的多农残检测。     

Carotenoid Composition of Jackfruit (<Emphasis Type="Italic">Artocarpus heterophyllus</Emphasis>), Determined by HPLC-PDA-MS/MS

Carotenoids are pigments responsible for the yellow-reddish color of many foods and are related to important functions and physiological actions, preventing several chronic-degenerative diseases. The objective of this study was to confirm the carotenoid composition of jackfruit by high-performance liquid chromatography connected to photodiode array and mass spectrometry detectors (HPLC-PDA-MS/MS). The main carotenoids were all-trans-lutein (24–44%), all-trans-β-carotene (24–30%), all-trans-neoxanthin (4–19%), 9-cis-neoxanthin (4–9%) and 9-cis-violaxanthin (4–10%). Either qualitative or quantitative differences, mainly related to the lutein proportion, were found among three batches of jackfruit. Since the fruits from batch A showed significantly lower contents for almost all carotenoids, it also had the lowest total carotenoid content (34.1 μg/100 g) and provitamin A value, whereas the total carotenoid ranged from 129.0 to 150.3 μg/100 g in the other batches. The provitamin A values from batches B and C were 3.3 and 4.3 μg RAE/100 g, respectively. The carotenoid composition of jackfruit was successfully determined, where 14 of the 18 identified carotenoids were reported for first time. Differences among batches may be due to genetic and/or agricultural factors.     

安吉白茶多糖对实验性糖尿病小鼠的降血糖作用研究

通过制备去甲肾上腺素致糖尿病小鼠模型及四氧嘧啶致高血糖小鼠模型,给正常小鼠、去甲肾上腺素致高血糖小鼠及四氧嘧啶致糖尿病小鼠连续灌胃安吉白茶多糖14 d后,取血测定血糖水平,以探讨安吉白茶多糖对正常小鼠、去甲肾上腺素致高血糖小鼠及四氧嘧啶致高血糖小鼠血糖水平及糖耐量（GT）的影响。结果显示,灌胃2周后,安吉白茶多糖对正常小鼠血糖水平影响较小,低、中、高剂量组与正常对照组相比均无显著意义(P>0.05);安吉白茶多糖能明显降低去甲肾上腺素所致糖尿病小鼠的血糖水平,低、中、高剂量组的血糖值与肾上腺素模型组比较,差异极显著(P<0.01)。且高剂量组降血糖效果优于低剂量组;安吉白茶多糖明显降低四氧嘧啶所致高血糖小鼠的血糖水平,三剂量组的血糖值与四氧嘧啶模型组比较,差异极显著(P<0.01)。三剂量均能降低实验性高血糖小鼠血糖,且随剂量增大,降血糖作用增强,以高剂量降糖作用最强。安吉白茶多糖在缓解糖尿病小鼠糖耐量降低方面作用显著,达到了药物组的治疗水平,但并不影响正常小鼠的血糖和糖耐量。     

信阳毛尖茶叶挥发性成分GC/MS分析

本文采用SDE蒸馏萃取方法提取信阳毛尖茶叶的挥发性成分,用气质联用仪及SE-54和强极性BPX70毛细色谱管柱进行分离分析比较,中等极性SE-54毛细色谱管柱分离效果较好,春茶挥发性成分中共分离并鉴定出47个峰;夏茶挥发性成分中共分离并鉴定出64个峰。对比夏茶与春茶在香气成分上的差异,综合评价春茶的香气品质优于夏茶。     

超高效液相色谱-质谱/质谱法同时测定蔬菜中7种磺胺的残留量

为建立超高效液相色谱-质谱/质谱法(UPLC-MS/MS)同时测定蔬菜中7种磺胺残留量的方法。样品用1%乙酸乙腈提取,以C18色谱柱分离待测物,采用多反应监测(MRM)离子扫描模式,外标法进行定量,线性良好,相关系数均大于0.999。结果显示：7种磺胺的检出限为0.000 4～0.000 6 mg/kg,样品添加回收率为67.5%～94.1%,相对标准偏差均少于5.3%(n＝6)。该方法简单快捷、定量准确,可满足多种蔬菜中7种磺胺的残留检测要求。     

超高效液相色谱-串联质谱法测定植物源调味料中氯虫苯甲酰胺残留

本研究建立了超高效液相色谱-串联质谱（UPLC-MS/MS）测定植物源调味料中氯虫苯甲酰胺残留量的分析方法。调味料样品经改进后的QuEChERS方法前处理,选择C₁₈超高效液相色谱柱进行分离,采用电喷雾离子源正离子模式、多反应监测方式进行采集,外标法定量。结果表明,方法在0.005~0.200 μg/mL范围内线性相关系数均优于0.999,加标回收率在70%~108%之间,相对标准偏差在1.9%~10%之间。方法检出限为0.002 mg/kg,定量限为0.005 mg/kg。该方法操作简便快速、灵敏、准确性高,适用于植物源调味料中氯虫苯甲酰胺的残留量检测。     

Anti-Inflammatory Effects of Mytilus coruscus Polysaccharide on RAW264.7 Cells and DSS-Induced Colitis in Mice

Considerable literature has been published on polysaccharides, which play a critical role in regulating the pathogenesis of inflammation and immunity. In this essay, the anti-inflammatory effect of Mytilus coruscus polysaccharide (MP) on lipopolysaccharide-stimulated RAW264.7 cells and a dextran sulfate sodium (DSS)-induced ulcerative colitis model in mice was investigated. The results showed that MP effectively promoted the proliferation of RAW264.7 cells, ameliorated the excessive production of inflammatory cytokines (TNF-α, IL-6, and IL-10), and inhibited the activation of the NF-κB signaling pathway. For DSS-induced colitis in mice, MP can improve the clinical symptoms of colitis, inhibit the weight loss of mice, reduce the disease activity index, and have a positive effect on the shortening of the colon caused by DSS, meliorating intestinal barrier integrity and lowering inflammatory cytokines in serum. Moreover, MP makes a notable contribution to the richness and diversity of the intestinal microbial community, and also regulates the structural composition of the intestinal flora. Specifically, mice treated with MP showed a repaired Firmicutes/Bacteroidetes ratio and an increased abundance of some probiotics like Anaerotruncus, Lactobacillus, Desulfovibrio, Alistipe, Odoribacter, and Enterorhabdus in colon. These data suggest that the MP could be a promising dietary candidate for enhancing immunity and protecting against ulcerative colitis.