液相色谱-电喷雾质谱联用检测蜂蜜中四种硝基呋喃类代谢物

介绍了高效液相色谱电喷雾多级质谱(LC/MSn) 同时快速、准确测定蜂蜜中呋喃西林、呋喃唑酮、呋喃它酮和呋喃妥英4种硝基呋喃类抗生素代谢物。硝基呋喃类代谢物在酸性条件下经过邻硝基苯甲醛衍生化, 液相萃取后经色谱分离, 利用二级质谱进行定性和定量。加标样品平均回收率达到64% ~79%, 定量下限(LOQ) 为0 1~1μg·kg-1, 检测限(LOD) 达到0 05~0 5μg·kg-1。该方法测定结果满足欧盟(EU)对进口动物源性食品中硝基呋喃类抗生素的残留要求。     

家蝇抗菌肽的分离纯化及生物学活性

将诱导家蝇提取的家蝇抗菌肽提取物，经凝胶过滤层析和离子交换层析，得到具有抗菌活性的单一峰，质谱结果显示抗菌肽分离物含有4种小肽，相对分子质量678．3～1017．2。家蝇抗菌肽对革兰氏阴性菌（大肠杆菌、巴氏杆菌）的抗菌活性优于革兰氏阳性菌（金黄葡萄球菌、枯草芽孢杆菌），对耐药性巴氏杆菌有较强的抗菌活性，对大肠杆菌的MIC为4．2～8．4mg／L，对耐药性巴氏杆菌的MIC为3．8～7．8mg／L。扫描电镜观察发现，家蝇抗菌肽通过损伤细胞壁使细胞质外流而达到杀菌的目的。家蝇抗菌肽对家兔、鸡、猪、小鼠、番鸭、鹅和家鸭红细胞无溶血反应和凝集反应。‘     

全细胞催化制备单糖酸及其鉴定

首次利用氧化葡萄糖酸杆菌全细胞催化方法,在液体振荡反应体系中分别制取葡萄糖、木糖、阿拉伯糖、半乳糖和甘露糖这5种植物单糖对应的单糖酸钙溶液。以高效阴离子交换色谱-脉冲安培检测器(HPAEC-PAD)对它们的纯度进行检测,并采用红外光谱(FT-IR)和电喷雾质谱(ESI-MS)进行了物质的结构解析与鉴定。结果显示,制备所得的5种单糖酸钙的离子色谱检测纯度均大于98%;它们的红外光谱在1600 cm-1处均有去质子化COO-基团的特征吸收;在电喷雾质谱中2种戊糖酸和3种己糖酸的特征离子峰[M-H]-分别为165.1和195.1,与理论值相符。     

高效液相色谱与电喷雾电离质谱联用测定婴儿配方奶粉中的牛磺酸和维生素

目的利用高效液相色谱与电喷雾电离质谱联用技术,建立一种同时测定婴儿配方奶粉中的牛磺酸和4种维生素(维生素B1、维生素B5、维生素B6、维生素PP)含量的分析方法。方法色谱条件采用RP-C18色谱柱,流动相为5mmol/L七氟丁酸和甲醇,梯度洗脱。质谱采用电喷雾正离子模式(ESI ),以马尿酸为内标定量。结果4种维生素和牛磺酸含量测定方法的线性关系良好(r=0.9996～0.9999,最低定量限10μg/L),前处理技术简单,用该法测定了婴儿配方奶粉中的牛磺酸和4种维生素的含量,回收率为99.1%～101.7%。结论本方法操作简便,精密度好,结果准确可靠。     

Disulphide structure of high-molecular-weight (HMW-) gliadins as affected by terminators

This study aimed at elucidating SS-bonds of HMW-gliadins (HGL) from wheat with the focus on terminators of glutenin polymerisation. HGL from wheat flour extracts non-treated or treated with the S-alkylation reagent N-ethylmaleinimide (NEMI) were compared. HGL from wheat flour Akteur were isolated, hydrolysed with thermolysin and the resulting peptides pre-separated by gel permeation chromatography and analysed by liquid chromatography/mass-spectrometry using alternating electron transfer dissociation/collision-induced dissociation. Altogether, 22 and 28 SS-peptides from samples without and with NEMI treatment, respectively, were identified. Twenty-six peptides included standard SS-bonds of α- and γ-gliadins, high-molecular-weight and low-molecular-weight glutenin subunits. Eleven SS-bonds were identified for the first time. Fifteen peptides unique to HGL contained cysteine residues from gliadins with an odd number of cysteines (ω5-, α- and γ-gliadins). Thus, gliadins with an odd number of cysteines, glutathione and cysteine had acted as terminators of glutenin polymerisation. Decisive differences between samples without and with NEMI treatment were not obvious showing that the termination of polymerisation was already completed in the flour. The two HGL samples, however, were different in the majority of ten peptides that included disulphide-linked low-molecular-weight (LMW) thiols such as glutathione and cysteine with the former being enriched in the non-treated HGL-sample.     

Localization of amino acids in germinated rice grain: Gamma-aminobutyric acid and essential amino acids production approach

Germinated rice is popularly consumed for its high gamma-aminobutyric acid (GABA) and bioactive compounds. Supporting information on how to germinate rice with high GABA content and essential amino acids is lacking. White and colored rough rice were germinated for 0, 24, 48, 72, 96, 120 and 144 h. GABA, GABA substrates and essential amino acids were also investigated using GC-MS and MALDI-MSI. GABA was more concentrated after germination and shifted into the coleoptile. High correlation was recorded between germination time and GABA (0.79–0.83, p ≤ 0.01) and glutamic acid (0.88–0.89, p ≤ 0.01). Highest rates of GABA and glutamic production were observed within 48 h of germination in both rice varieties (26.12 and 34.28 mg/100g) and reached maximum value at 96 h (31.36 and 38.75 mg/100g). Colored rice germination showed higher GABA, GABA substrates and deficient amino acids than white rice. GABA and essential amino acids drastically increased after germination, supporting the consumption of germinated rice as a functional food.     

小尺度双网格荷电雾化燃烧器热损失特性研究

以无水乙醇为燃料,运用荷电雾化技术,实验研究了锥-射流喷雾模式下双网格燃烧器的燃烧与热损失特性。结果表明,在当量比Φ为0.85~1.40区间内燃烧稳定,圆形片状火焰附着于燃烧网格附近,火焰直径与燃烧器内径相当。火焰温度、燃烧效率均随当量比的增大先上升后下降,在当量比Φ=1时分别达到最大值1 197.38 K、93.26%。尾气温度随当量比的增大而降低,壁面热损失随当量比增大而增加。壁面热损失与燃料完全燃烧释放热量比例为27.25%~33.08%,其中辐射热损失略高于对流热损失。燃烧器热效率在当量比Φ≤1下可达69%。双网格燃烧器可实现小尺度条件下液体乙醇的良好喷雾、蒸发与燃烧。     

电喷雾萃取及电离质谱法分析大豆水提液快速鉴别种子活力

为快速评价大豆种子活力,该文以人工加速老化后的大豆种子为原料,采用电喷雾萃取电离质谱（extractive electrospray ionization-mass spectrometry,EESI-MS）直接检测不同活力大豆种子水提液,获得其正离子模式下指纹图谱,结合主成分分析（principal component analysis,PCA）、聚类分析（cluster analysis,CA）和判别分析（discriminant analysis, DA）,建立鉴别大豆种子活力的方法。结果表明,在正离子模式下,电喷雾萃取电离质谱结合多变量分析方法可以有效鉴别不同活力大豆种子。主成分分析提取了前3个主成分因子,累计贡献率达到94.80%,聚类分析和判别分析的正确率都为100%,对外部验证样本进行判别分析,正确率为95%。电喷雾萃取电离质谱能快速鉴别不同活力大豆种子,为种子活力检测提供了一种快速、准确、高效的新方法。     

亚麻籽中开环异落叶松树脂酚二葡萄糖苷的测定——高效液相色谱-二极管阵列检测 电喷雾质谱法

    采用高效液相色谱-二极管阵列检测-电喷雾质谱(HPLC-PAD-ESI-MS)法对开环异落叶松树脂酚二葡萄糖苷(SDG)进行定性和定量检测,研究方法的精密度、稳定性、定量检测限及加样回收率,并考察样品制备方法对定量检测结果的影响.采用Sephadex LH-20柱色谱分离制备SDG对照品,并用1H-NMR与13C-NMR对其进行表征.HPLC-PAD-ESI-MS检测所得紫外及电喷雾质谱信息与SDG结构相符.以自制的SDG(纯度96.6%)为对照,采用HPLC绘制定量标准曲线,方法精密度较高(RSD为1.36%),稳定性好(1周后RSD为1.21%),定量检测限较低(LOQ为3.4 mg·L-1),加样回收率达(99.7±3.2)%.此外,制样时采用碱法水解与混合溶剂提取,不仅节省时间,还更充分地提取了SDG.说明用HPLC-PAD-ESI-MS法栓测亚麻籽中的SDG方便省时,准确可靠.     

Metabolic signature of spent culture media shows lipid metabolism as a determinant of pregnancy outcomes

In the present study, we investigated the spent culture media of in vitro produced (IVP) bovine embryos which did (group Pregnant) or did not (group Non-pregnant) establish pregnancy after transfer. For that purpose, IVP embryos on D5 were transferred to individual droplets for the last 48 h of culture. Embryos at the blastocyst stage were then transferred to synchronized recipients, while respective culture media drops were collected and evaluated individually. The list of metabolites present in spent culture media was obtained by electrospray ionization mass spectrometry (ESI-MS) and analysed with Metaboanalyst® to characterize the metabolic profile of each group. The spectrometric analysis showed that pathways related to lipid metabolism, particularly fatty acids degradation via beta-oxidation, were more present in the Pregnant group whereas no significant pathway was identified in the group Non-pregnant. By using this method, we were able to identify a metabolic signature in culture media that allows for a better comprehension of preferential metabolic routes taken by the most viable embryos. These findings offer great insights into the biochemistry of embryo development and reveal a potential target for the development of better-quality IVP systems, as well as tools to identify bovine embryos with greater chances to establish and maintain pregnancy.