铜陵白姜精油分析研究

利用水蒸气蒸馏法和同时蒸馏-萃取法(SDE)萃取铜陵白姜姜精油,并通过GC/MS方法进行定性、定量分析。结果显示,SDE法能够有效地提取到姜精油,经GC/MS分析鉴定出87种组分。以色谱峰面积归一化法测定各成分的相对百分含量,含量最高的是姜烯(21.91%),其次是乙酸香叶酯(12.45%)、β-倍半水芹烯(11.76%)、金合欢烯(11.73%)。乙酸香叶酯在铜陵白姜中含量较高。     

In vitro ruminal biohydrogenation of eicosapentaenoic (EPA), docosapentaenoic (DPA), and docosahexaenoic acid (DHA) in cows and ewes: Intermediate metabolites and pathways

A great deal of uncertainty still exists about intermediate metabolites and pathways explaining the biohydrogenation (BH) of 20- and 22-carbon polyunsaturated fatty acids (PUFA). Therefore, this study was conducted to provide further insight into the ruminal metabolism of 20:5 n-3 (EPA), 22:5 n-3 (DPA), and 22:6 n-3 (DHA), the main n-3 PUFA present in the marine lipids used in dairy ruminant feeding, and to examine potential differences between bovine and ovine. To meet this aim, we investigated the 20- and 22-carbon metabolites accumulated during in vitro incubation of EPA, DPA, and DHA with rumen inocula from cows and ewes. The PUFA were added at a dose of 2% incubated dry matter and digesta samples were analyzed after 24 h of incubation using complementary gas-liquid chromatography of fatty acid methyl esters and gas chromatography-mass spectrometry of 4,4-dimethyloxazoline derivatives. Results suggested that the main BH pathway of EPA and DPA would proceed via the reduction of the double bond closest to the carboxyl group (cis-5 in EPA and cis-7 in DPA); curiously, this mechanism seemed of much lower importance for DHA. Thus, DPA would not be a major intermediate product of DHA and their BH might actually follow separate pathways, with the accumulation of numerous unique metabolites in each case. A principal component analysis supported this hypothesis, with a clear separation between PUFA treatments in the score and loading plots. Within EPA and DPA groups, cow and ewe samples loaded separately from each other but not distant. No conjugated 20:5, 22:5, or 22:6 isomer compatible with the initial product of EPA, DPA, or DHA metabolism, respectively, was identified in the ruminal digesta, although this would not unequivocally exclude their transient formation. In this regard, results from DPA incubations provided the first indication that the metabolism of this very long chain PUFA may involve the formation of conjugated double bond structures. The BH of EPA, DPA, and DHA resulted in the appearance of several tentative trans-10–containing metabolites, showing a general trend to be more abundant in the digesta of ewes than in that of cows. This finding was speculated to have some relationship with the susceptibility of dairy sheep to marine lipid-induced milk fat depression. Differences in the relative proportion of intermediate products would also suggest an influence of ruminant species on BH kinetics, with a process that would likely be slower and less complete in cows than in ewes.     

XPS、AFM和ToF-SIMS的工作原理及在植物纤维表面分析中的应用

介绍了先进的表面分析仪器化学分析电子能谱(XPS)、原子力显微镜(AFM)、含飞行时间分析器的二次离子质谱仪(ToF-SIMS)的工作原理,回顾了近年来它们在植物纤维表面分析中的成功应用,综合利用XPS、AFM及ToF-SIMS方法,可分析和解决制浆造纸过程中的现象和问题。     

吹扫捕集气质联用法测定水中吡啶

建立了吹扫捕集气质联用法测定水中吡啶的方法,优化了吹扫条件,用自动进标样的方法绘制工作曲线,方法的检出限为0.08μg/L,相对标准偏差在1.5%～5.1%之间,方法用于地表水、生活污水和化工废水中吡啶的测定,进行了加标回收实验,回收率在82.5%～102.5%之间。     

Application of electrospray ionization ion trap/time-of-flight mass spectrometry for chemically-synthesized small RNAs

In this study, we have demonstrated an accurate and rapid small RNA analytical method with both sequence determination and detailed modification analysis by electrospray ionization-ion trap/time-of-flight mass spectrometry (ESI-IT/TOFMS). To develop this ideal method, we have examined the performance of ESI-IT/TOFMS using various chemically-synthesized model sequences of modified or unmodified microRNAs (miRNAs). The deconvoluted mass of a 22-nucleotide (nt) miRNA was obtained from a multiply charged precursor ion (MS(1)). The ion exhibited high mass accuracy (< 7 ppm) and high mass resolution (a value of m/Δm=10,000) and was therefore very useful in RNA composition assignment. The optimized MS(2) method using ion trap collision-induced dissociation, as well as automatic annotation analysis of product ions based on the accurate mass information, enabled the precise sequencing determination of intact miRNAs. Further, the detailed structural analysis of 3'-terminal modified nucleic acid in intact methylated miRNA was carried out using the MS(3) capability of the hybrid IT/TOFMS. The direct infusion method also provided a high throughput and good sensitivity because the analytical time and sample concentration needed in a series of experiments with reliable data were only 3 min and 100 nM, respectively. This study provides a novel approach for characterizing the intact chemically-synthesized small RNA without chemical and enzymatic digestions and would be widely applicable for the structural analysis of complicated modified small RNAs.     

Nutritional supplements to increase muscle mass.

Although nutritional supplements purported to increase muscle mass are widely available at health food stores, gyms, by mail order, and over the Internet, many of these supplements have little or no data to support their claims. This article reviews the theory and research behind popular nutritional supplements commonly marketed as muscle mass builders. Included are the minerals chromium, vanadyl sulfate, and boron, the steroid hormone dehydroepiandrosterone (DHEA), beta-methyl-hydroxy-beta-methylbutyrate (HMB), creatine, protein supplements, and amino acids. Research has shown that chromium vanadyl sulfate, and boron do not appear to be effective in increasing lean body mass. The few studies examining DHEA have not supported the claim of increased muscle gain. Preliminary work on HMB supports an anticatabolic effect, but only one human study is currently available. Many studies reported increased body mass and several have reported increased lean body mass following creatine ingestion. This weight gain is most likely water retention in muscle but could also be due to some new muscle protein. Although athletes have a greater protein requirement than sedentary individuals, this is easily obtained through the diet, negating the use of protein supplements. Studies on amino acids have not supported their claim to increase growth hormone or insulin secretion. Nutritional supplements can be marketed without FDA approval of safety or effectiveness. Athletes who choose to ingest these supplements should be concerned with unsubstantiated claims, questionable quality control, and safety of long-term use.     

Monitoring Phenolic Composition of Maturing Maize Stover by High Performance Liquid Chromatography and Pyrolysis/Gas Chromatography/Mass Spectrometry*

Maize stovers collected every 14 days over an 84-day growth period were subjected to high-performance liquid chromatography with electrochemical detector (HPLC-ED) and pyrolysis/gas chromatography/mass spectrometry (PY/GC/MS) in order to monitor changes in the phenolic composition. Prior to HPLC-ED analyses, ground samples were sequentially extracted with (i) methanol, (ii) 0·1M sodium hydroxide and (iii) 2M sodium hydroxide in the presence of nitrobenzene to separate, respectively, free phenolic monomers, alkali-labile phenolic monomers and alkali-resistant lignin. In turn, solution (ii) was treated with alkaline nitrobenzene to obtain (iv) alkali-labile lignin. Pyrolysis was carried out on ground native samples by using a platinum heated filament pyrolyser. Increases in the absolute phenolic concentrations in the residues of 0·1M sodium hydroxide extraction and in the ratio of alkali-resistant lignin vs total lignin were observed by HPLC-ED during the first 28–42 days of maturation, reaching a steady level in the remaining maturation period. A linear increase of syringyl units vs guaiacyl units was for found the alkali-resistant lignin fraction over the entire period of maturation. Similar trends were showed by PY/GC/MS with regard to relative lignin content and syringyl/guaiacyl ratio. Both techniques showed their usefulness to gauge changes in the phenolic composition during the lignification process.     

固相萃取-气相色谱-质谱联用法测定啤酒大麦中抗蚜威、乙草胺、三唑酮的残留量

研究了气相色谱/质谱法测定啤酒大麦中杀虫剂抗蚜威、除草剂乙草胺、杀菌剂三唑酮3种农药残留的分析检测方法。样品以丙酮作为提取剂,采用超声波清洗器和旋涡混合器混合提取啤酒大麦中的农药残留,经500mg、3mL SupelcleanTML C-18固相萃取柱净化。同时采用SIM的扫描模式,有效地去除了一些杂质的干扰,提高了分析的选择性。该方法的添加回收率在88%～106%,相对偏差小于5.61%,检测限0.010～0.020μg/kg,可相对快捷地检测啤酒大麦中抗蚜威、乙草胺、三唑酮。     

Fatty acid intake and milk fatty acid composition of Holstein dairy cows under different grazing strategies: Herbage mass and daily herbage allowance

The objective of this study was to investigate the effect of level of 1) pregrazing herbage mass (HM) and 2) level of daily herbage allowance (DHA) on the performance and fatty acid (FA) composition of milk from grazing dairy cows. Sixty-eight Holstein-Friesian dairy cows were allocated to either a high or low pregrazing HM (1,700 vs. 2,400 kg of DM/ha; >40 mm), and within HM treatment, cows were further allocated to either a high or low DHA (16 vs. 20 kg of DM/d per cow; >40 mm) in a 2 × 2 factorial design. Pregrazing HM did not affect dry matter intake (17.5 ± 0.75 kg/d), milk production (22.1 ± 0.99 kg/d), milk composition (milk fat, 3.88 ± 0.114%; milk protein, 3.28 ± 0.051%), body weight (525 ± 16 kg), or body condition score (2.65 ± 0.064). Increasing DHA increased dry matter intake (+1.5 kg/d) but did not affect any other variable measured. Cows grazing the low HM or high DHA had a higher daily intake of total FA (+0.12 and +0.09 kg/d, respectively, for the low HM and high DHA), α-linolenic acid (LNA; +0.08 and +0.05 kg/d, respectively, for the low HM and high DHA), and linoleic acid (+0.01 for both the low HM and high DHA) compared with either the high HM or low DHA. Milk conjugated linoleic acid (cis-9, trans-11 isomer) was not affected by treatment (13.0 ± 0.77 g/kg of total FA); however, large variation was recorded between individual animals (range from 5.9 to 20.6 g/kg of total FA). Milk concentrations of LNA were higher for animals offered the low HM (5.3 g/kg of total FA), but across treatments, milk concentrations of LNA were low (4.9 ± 0.33 g/kg of total FA). The present study indicates that changes in HM and DHA do not have a great effect on the milk FA composition of grazing dairy cows. Further enhancement of the beneficial FA content in milk purely from changes in grazing strategy may be difficult when pasture quality is already high.     

Identification of the compound in a potent cranberry juice extract that inhibits lipid oxidation in comminuted muscle

An extract prepared from cranberry juice powder using a mixture of chloroform and methanol was particularly effective at inhibiting lipid oxidation in mechanically separated turkey (MST), providing more than 3 weeks of additional stability during −4 °C storage at a usage level of 0.1% (wet weight basis). The chloroform extract was fractionated by flash chromatography (FC) and analysed using reverse-phased high performance liquid chromatography (RP-HPLC) with UV/vis diode array detection to identify the component(s) present in the fractions. One of the five fractions obtained was effective in delaying the formation of lipid peroxides and thiobarbituric acid reactive substances (TBARS) in MST, while the remaining fractions had little to no inhibitory action. Mass spectrometry (MS) analysis indicated the presence of two flavonols, quercetin and quercetin-3-O-(6″-benzoyl)-β-galactoside in the inhibitory fraction. This fraction (containing quercetin at 467 μmol/kg MST) inhibited lipid oxidation in MST similarly to pure quercetin added to MST at the same concentration. This indicated that quercetin accounted for all or nearly all of the inhibitory capacity in the chloroform extract.