野巴旦杏营养成分及苦杏仁苷的测定

对新疆特有资源野巴旦杏的多种营养成分和药用成分进行测定。分别用索氏抽提法、微量凯氏定氮法测定野巴旦杏中脂肪、蛋白质,用氨基酸分析仪测定多种氨基酸含量,原子吸收法测定多种元素,紫外法及反相高效液相法测定天然苯甲醛及苦杏仁苷。测定结果表明野巴旦杏中含脂肪53.09%、蛋白质24.2%、氨基酸总量14.57%,并含多种微量元素,脱脂样品中苯甲醛及苦杏仁苷含量分别为1.363%、5.320%。野巴旦杏具有很好的利用开发价值。     

Determination of total nitrogen and cyanide nitrogen in cassava

Heating of intact cassava leaves causes liberation of hydrogen cyanide. This phenomenon appears to be caused by β-glucosidase-catalysed decomposition of the cyanogenic glycosides linamarin and lotaustralin. Because of these losses, many previously determined values for total nitrogen in cassava (and other cyanogenic plants) are probably in error as plant materials used for Kjeldahl determinations are often dried at 70–90°C. Liberation of cyanide from intact cassava leaves by heating at 80°C is more complete than liberation by the homogenisation methods commonly used. Homogenisation of cassava leaf tissues with liquid nitrogen or dry ice gives somewhat lower values, and these materials are often not readily available in areas where cassava is studied. The basis of a relatively simple procedure for the isolation of hydrogen cyanide from cassava leaves is suggested.     

高效液相色谱-质谱联用测定乳制品中6种四环素类抗生素

建立了乳制品中6种四环素类抗生素残留的高效液相色谱-电喷雾离子阱质谱联用测定方法。该方法采用多反应监测正离子模式，可一次对6种四环素类抗生素进行定性和定量分析。该方法的检出限0．5-4．0μg/L，测定低限牛奶0．6-4.5μ/L，乳粉为6．0-45．0μg/kg，线性范围4．0-100．0μg／L，加标回收率56．1％-104．9％，相对标准偏差为2．5％-15．0％。该法具有样品预处理简单，灵敏度高，分析时间短等优点。     

Extraction, Identification, and Quantification of Flavonoids and Phenolic Acids in Electron Beam-Irradiated Almond Skin Powder

ABSTRACT:  The effect of electron beam irradiation doses from 0 to 30 kGy on extraction yield and phenolic compounds was evaluated in almond skin phenolic extracts (ASPE). Total soluble phenols and distribution of phenolic compounds from acidified methanol ASPE and 52% methanol ASPE were quantified using Folin–Ciocalteau method, liquid chromatography with diode array and fluorescence detection, and negative ion electrospray-mass spectrometry. Electron beam irradiation increased extraction yield by as much as 23%, with the greatest increase observed in the acidified methanol ASPE. Irradiated samples extracted with acidified methanol also exhibited an increase in extractable phenols (Folin–Ciocalteau) and total HPLC-resolved phenolics at all irradiation doses. Samples extracted with 52% methanol exhibited an increase at 10 and 20 kGy, but a 31% decrease at 30 kGy. An increase in aglycones respective to their glycosides was not observed with irradiation. Therefore, the increase in phenolics was attributed to release of phenolics from their cellular matrix.     

Determination of malachite green and crystal violet in processed fish products

This paper presents analysis of malachite green (MG) and crystal violet (CV) residues in processed fish products. Samples were homogenized and extracted with ammonium acetate buffer and acetonitrile. The extracted residues were partitioned into dichloromethane, in situ oxidized to chromic forms with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone, and cleaned up on neutral alumina and propylsulfonic acid cation-exchange solid-phase extraction (SPE) cartridges. MG and CV were determined at 618 and 588 nm using HPLC with a visible detector (LC–VIS) and confirmed by LC–electrospray ionization tandem mass spectrometry (LC–ESI–MS/MS). The recoveries were as follows: MG (74.8–83.8%), LMG (80.0–88.4%), CV (68.6–73.9%), and LCV (85.5–90.0%). The method modified in this study has been evaluated by application in-house to a survey of 253 processed fish products. As a result of monitoring, MG and CV were positive in one shrimp and one eel sample, respectively. Our results showed that regular monitoring of these antibiotic residues is recommended for protection of public health.     

An LC–ESI–MS/MS method for residues of fluoroquinolones,sulfonamides, tetracyclines and trimethoprim in feedingstuffs: validation and surveillance

ABSTRACT

An increasing concern about food safety has been observed over the years. The presence of drugs residues in food is one of the major subjects of research in food safety. Feedingstuffs can be responsible for carryover into the food chain of residues of several drugs. This paper describes the development, validation and application of a fast and simple method for analysis of 24 antibiotic residues in feedingstuffs for cattle, pigs and poultry. Analytes include compounds from different antimicrobials classes, such as sulfonamides (sulfadiazine, sulfamethazine, sulfamethoxazole, sulfaquinoxaline, sulfachlorpyridazine, sulfadoxine, sulfadimethoxine, sulfizoxazole, sulfamerazine and sulfathiazole), fluoroquinolones (ciprofloxacin, enrofloxacin, norfloxacin, danofloxacin, difloxacin, sarafloxacin, flumequine, nalidixic acid and oxolinic acid), tetracyclines (tetracycline, doxycycline, oxytetracycline and chlortetracycline) and trimethoprim. Samples were extracted with methanol:water (70:30) 0.1% formic acid, followed by clean-up steps using centrifugation, low-temperature purification (LTP) and ultracentrifugation. Instrumental analysis was performed using liquid chromatography coupled to tandem mass spectrometry. Chromatographic separation was achieved using a C18 column and a mobile phase composed of acetonitrile and water, both with 0.1% formic acid. Validation parameters such as limit of detection (LOD), limit of quantification (LOQ), selectivity, linearity, accuracy, precision, decision limit (CCα) and detection capability (CCβ) were determined and meet the adopted criteria. LOD and LOQ were set to 30 and 75 µg kg^?1, respectively. Inter-day precision were in the range from 4.0 to 11.1%, and linearity provides values of r² above 0.95 for all analytes. The optimised method was applied to the analysis of more than 1500 real samples within the period 2012–2017. Non-compliant results were discussed and classified in terms of analytes, feed types and target species. Multivariate analysis of the data was performed using principal component analysis.     

Proteome analysis of Pithecellobium dulce seeds using two‐dimensional gel electrophoresis and tandem mass spectrometry

BACKGROUND: Pithecellobium dulce Benth. belongs to the Leguminosae family, which contains several members that are important components of human diets owing to their high protein content and quality. In this study the seed proteins from P. dulce were separated and identified using two‐dimensional gel electrophoresis (2‐DE) and mass spectrometry respectively. RESULTS: The 2‐DE protein map revealed a total of 317 distinct protein spots, including a cluster of about 12 proteins located in the region of pI 5–6 with molecular masses of 55–97 kDa that accounted for more than 50% of the total proteins. Ninety‐six of the most abundant protein spots were analysed using nano liquid chromatography/tandem mass spectrometry (LC/MS/MS), from which 27 were successfully identified through the query of acquired tandem mass spectral data used in MASCOT searching against a custom legume protein database. A further four proteins from the highly abundant protein cluster were putatively identified using mass spectrometry‐driven BLAST (MS‐BLAST) homology searches. CONCLUSION: This research has generated a 2‐DE proteome reference map for P. dulce seeds and used LC/MS/MS to characterise the proteins. The identification of proteins from P. dulce was carried out using the sequence database successively for MASCOT and MS‐BLAST homology‐based searches. Copyright © 2009 Society of Chemical Industry     

Baseline levels of melamine in food items sold in Canada. II. Egg,soy, vegetable,fish and shrimp products

A variety of egg-containing, soy-based, fish, shrimp and vegetable products sold in Canada were analysed for melamine (MEL) using a sensitive solid-phase extraction LC–MS/MS analytical method. MEL was detected above the method quantification limit of 0.004 mg/kg in 98 of the 378 samples analysed. Concentrations in the various food product groups ranged 0.00507–0.247 mg/kg (egg-containing items), 0.00408–0.0479 mg/kg (soy-based meat substitutes), 0.00409–1.10 mg/kg (fish and shrimp products), and 0.00464–0.688 mg/kg (vegetable products). MEL was detected less frequently in egg- and soy-containing products. The presence of MEL in most of the Canadian Total Diet Study shrimp composites collected after 2001 suggested the residues in shrimp were caused by a relatively recent exposure to MEL. All concentrations of MEL reported were lower than the 2.5 mg/kg interim standard established for MEL in items containing milk and milk-derived ingredients and the respective maximum residue limits for cyromazine and its metabolite, melamine, in vegetables set by the Canadian Government (2009; http://www.hc-sc.gc.ca/fn-an/securit/chem-chim/melamine/qa-melamine-qr-eng.php#8). The consumption of foods containing these low levels of MEL does not constitute a health risk for consumers.     

超声波处理对红葡萄酒总酚、总黄酮含量及自由基清除活性的影响

应用超声波处理红葡萄酒,探讨超声因素（超声频率,超声功率,超声处理温度,超声时间）对红葡萄酒中总酚、总黄酮含量及自由基清除活性的影响。结果表明超声处理会使红葡萄酒总酚含量、总黄酮含量与自由基清除活性显著降低（p<0.05）。超声处理红葡萄酒后,其抗氧化活性与其总酚含量呈高度正相关,回归方程为y=0.0270x+38.806（R2=0.9007,p<0.01）;其抗氧化活性与其总黄酮含量亦存在一定线性关系,回归方程为y=0.0592x+37.357（R²=0.4970,p<0.05）。在本文实验条件下根据实验结果可以推知,超声处理后红葡萄酒自由基清除活性的降低,部分是由于总酚含量和总黄酮含量降低所引起的。      

Influence of aflatoxin in Nuruk on the safety of starch-based alcoholic beverage

Nuruk is a fermentation agent used to manufacture alcoholic beverages, which contains a variety of microorganisms. Most microorganisms in Nuruk are useful for the production of alcoholic beverages; however, Nuruk can be infected with Aspergillus flavus, which produces aflatoxin (AF). Therefore, this study analyzed total AF concentrations in Nuruk, the transfer of AF from Nuruk to alcoholic beverages, and AF-producing microorganisms to determine the safety of alcoholic beverages with respect to this toxin. ELISA showed that total AF levels in 14 of 61 Nuruk samples exceeded 15 ppb, the Korean permissible level in cereal products. In alcoholic beverages produced with Nuruk containing AF levels >15 ppb, only AF G₁ was detected, at a level of 0.3 ppb, and the transfer ratio of AF G₁ was approximately 1.2% to 1.3%. The dominant genera in Nuruk were Aspergillus and Rhizopus. Among 30 strains belonging to Aspergillus, 10 produced only AF B₁ at levels of 0.1 to 2.4 ppb after incubation at 25 °C for 8 days on potato dextrose agar plates. Although AF in Nuruk was rarely transferred to alcoholic beverages and the aflatoxigenic strains were found to possess poor AF-producing capacity, further efforts to reduce AF in Nuruk are needed to ensure the safety of alcoholic beverages.     

Non‐galloylated and galloylated proanthocyanidin oligomers in grape seeds from Vitus vinifera L. cv. Graciano,Tempranillo and Cabernet Sauvignon

Non‐galloylated and galloylated flavan‐3‐ol composition in seeds from Vitis vinifera L. var. Graciano, Tempranillo and Cabernet Sauvignon grapes harvested in 2000, 2001 and 2002 at the same geographical area were determined using normal‐phase HPLC coupled with electrospray ionization mass spectrometry (LC/ESI‐MS) detection. Non‐galloylated and monogalloylated flavan‐3‐ols up to octamers, and di‐, and trigalloylated flavan‐3‐ols up to heptamers were identified in all grape seeds. Comparisons of the flavan‐3‐ol composition in three grape varieties harvested in three different years indicate that levels of non‐galloylated flavan‐3‐ols decrease as the degree of polymerization increased, whereas the monogalloylated dimers were present in the highest levels in all varieties and vintages. The levels of other monogalloylated flavan‐3‐ols varied in different vintages. Tempranillo contained the lowest levels of non‐galloylated and monogalloylated flavan‐3‐ols, whereas Graciano contained the highest levels, with the exception of non‐galloylated flavan‐3‐ols in vintage 2001, and non‐galloylated monomers in vintages 2000 and 2002. Grape seeds from vintage 2000 contained the highest levels of both non‐galloylated and galloylated structures. Statistical analyses indicate that the distribution of the flavan‐3‐ols is primarily determined by genetic factors and is also strongly influenced by climate conditions. Copyright © 2006 Society of Chemical Industry     

Degradation Kinetics of Jujuboside a by Rat Intestinal Flora and Identification of the Metabolites by HPLC-Ms/Ms

Jujuboside A (JuA) is a representative saponin with significant sedative and hypnotic effects. Up to now, there were many arguments on its metabolic mechanism. In this study, a high performance liquid chromatography-tandem mass spectrometry (MS/MS) method was developed for investigating the degradation characteristics of JuA incubated with rat feces. With the method, the degradation kinetics of JuA was studied. The results showed JuA decomposed rapidly. It could decompose nearly 100% in only 4–6 h. The degradation regularity was consistent with the first dynamic process. In addition, seven metabolites were determined and identified to be the serial hydrolysis products of JuA. The results revealed that gastrointestinal microbiota played an indispensable role in the metabolic process of JuA. JuA may be a supplier of sugars under the hydrolysis effect induced by the bacterial enzymes. At the same time, its aglycone was produced as a by-product, which could be easier to be absorbed into the body to perform its specific bioactivities.     

糖化工艺对麦汁中游离嘌呤碱基含量的影响

采用优化的反相离子对色谱法,对麦汁中4种嘌呤碱基和3种嘌呤核苷进行检测:7种化合物的平均回收率为95.13%～102.12%,相对标准偏差为0.10%～6.55%。设计正交实验利用SPSS18.0软件分析糖化工艺对麦汁中游离嘌呤碱基含量的影响,结果显示:料水比(A)、糖化温度(B)、蛋白质休止时间(C)和蛋白休止温度(D)均具有显著性影响,主次顺序为B>A>C>D,优化工艺为料水比1:2.5,45℃保温50min,升温至62℃,麦汁中游离嘌呤碱基含量从43.82mg/L提高到61.39mg/L,同时,嘌呤核苷从55.46mg/L降低为29.21mg/L。      

Fast analysis of glufosinate,glyphosate and its main metabolite,aminomethylphosphonic acid,in edible oils,by liquid chromatographycoupled with electrospray tandem mass spectrometry

ABSTRACT

A method has been developed for the rapid, specific, accurate, precise and sensitive determination of glufosinate, glyphosate and its major metabolite, aminomethylphosphonic acid, in edible oils, by liquid chromatography coupled to tandem mass spectrometry. Oils were extracted with acidified water (1% formic acid), and the extracts were directly injected into an LC using a Hypercarb column as the stationary phase. The analytes were eluted by a mobile phase of methanol and water containing 1% acetic acid, and they were ionised by electrospray ionisation in negative ion mode. The method was validated and limits of quantification ranged from 5 μg kg^?1 (aminomethylphosphonic acid) to 10 μg kg^?1 (glyphosate and glufosinate). Three concentrations (10, 50 and 100 μg kg^?1) were selected to perform recovery studies. Mean recoveries ranged from 81.4% to 119.4%. Intra and inter-day precision were lower than 19%. Different edible oils were analysed, and no residues of the studied herbicides were detected above limits of quantification.     

A preliminary study of presence of resveratrol in skins and pulps of European and Japanese plum cultivars

BACKGROUND: Resveratrol is a polyphenol with health properties being mainly present in the skins of several foods. However, any study has been carried out to analyze the presence of this stilbene in the plum fruit from the genus Prunus in European and Japanese cultivars. RESULTS: The analysis of resveratrol from the skin in different cultivars of plums from Spanish markets with liquid chromatography coupled to ultraviolet (LC‐UV) detector with subsequent confirmation by LC‐MS/MS has been demonstrated that contents of this compound in plums ranged from 0.1 to 6.2 µg/g. CONCLUSIONS: Values of resveratrol in European plum cultivars is higher than in Japanese cultivars. Copyright © 2012 Society of Chemical Industry     

Corticosteroids in liver and urine in Sicilian cattle by a LC-MS/MS method

The presence of corticosteroid residues was assessed in urine and liver samples from livestock of Sicily. A total of 630 bovine samples were collected from farms and slaughterhouses. The samples were analysed using solid-phase extraction (SPE) coupled with ultra-performance liquid chromatography tandem mass spectrometry (UHPLC–MS/MS). All the corticosteroids found were under the maximum residue limit imposed by Commission Regulation (EC) 37/2010. About 4% of liver samples showed dexamethasone levels above the limit of detection (LOD), with a mean of 1.5 ± 0.2 µg kg^?1. Betamethasone was found only in seven liver samples, with a mean of 1.6 ± 0.1 µg kg^?1. Furthermore, prednisolone and prednisone were found only in urine and liver samples from slaughterhouse, probably related to the high rate of stress for bovines. These results suggest good control practices adopted by Sicilian farms, able to ensure the quality of food products.