高效液相色谱-串联质谱法测定玉米及其制品中隐蔽型伏马毒素

目的 建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)检测玉米及玉米制品中隐蔽型伏马毒素的方法。方法 样品中加入伏马毒素B1和B2的稳定同位素内标, 用2 mol/L氢氧化钠溶液进行水解, 使隐蔽型及游离型伏马毒素一并转变为水解型伏马毒素, 用乙酸乙酯萃取水解型伏马毒素。色谱分离采用0.1%甲酸(A)和甲醇(B)作为流动相进行梯度洗脱, 质谱采用正离子扫描(positive ion electrospray ionization, ESI+)、多反应监测模式(multiple reaction monitoring, MRM)对水解型伏马毒素B1和B2(hydrolyzed fumonisin B1 and B2, HFB1和HFB2)的定量离子和定性离子进行监测。另取一份平行样品, 根据国家标准GB 5009.240-2016第二法测定其中的游离型伏马毒素含量。样品中隐蔽型伏马毒素的含量(按伏马毒素当量计)通过水解型伏马毒素减去游离型伏马毒素含量计算而得。结果 本方法在15 min内完成HFB1和HFB2及其稳定同位素内标的高效液相色谱-串联质谱分离分析。HFB1和HFB2在50、100和1000 μg/kg添加水平的回收率为89.1%~109.2%, 相对标准偏差为3.3%~12.2% (n=6), 方法定量限为15~20 μg/kg。结论 该方法准确、灵敏, 前处理简单, 适合测定玉米及其制品中的隐蔽型伏马毒素。     

液相色谱串联质谱-同位素内标法快速测定 玉米面中的伏马菌毒素

目的建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)以同时测定玉米中3种伏马菌素(FB1,FB2 and FB3)。方法试样经50%乙腈/水溶液超声提取,离心,多功能柱净化后液相色谱/串联质谱仪直接测定,13C34-FBs内标法定量。结果加标回收率范围为75.9%~108.2%,方法检测限在0.39~0.58μg/kg之间。将本方法用于实际样品分析,67%的玉米面中同时检出3种伏马菌素(FB1,FB2 and FB3)。结论此方法简便快速,灵敏度较高,可以用于准确定量检测粮食中的伏马菌素。     

超高效液相色谱-串联质谱法快速测定稻谷和玉米中伏马毒素

目的 建立了同位素稀释-超高效液相色谱串联质谱法测定稻谷和玉米中伏马毒素。方法 样品加入同位素内标后用50%乙腈水溶液(含1%甲酸)提取,采用ZORBAX Eclipse Plus C18 色谱柱分离,以甲醇-0.1%甲酸水溶液为流动相,梯度洗脱,质谱采用电喷雾电离,负离子模式下,以多反应监测模式(MRM)检测,内标法定量。结果 FB1,FB2和FB3在0.5~100.0μg/L范围内线性关系良好,相关系数均大于0.995,检出限均为1.0μg/kg。在5.0、50.0、500.0μg/kg三个加标浓度水平下,FB1,FB2和FB3的回收率在82.5~107.1%之间,RSD为3.9%~6.2%(n=5)。结论 该方法简单快速,定性定量准确,有效降低了背景干扰,可用于粮食中伏马毒素的检测。     

谷物中伏马菌素B1酶联免疫分析法的建立

以匙孔血蓝蛋白(KLH)为载体,采用碳化亚二胺法人工合成伏马菌素B1(FB1)抗原FB1-KLH,免疫大白兔获得特异性良好的抗FB1 多克隆抗体;在多克隆抗体的基础上建立伏马菌素B1 的间接竞争酶联免疫吸附分析方法,该方法IC50 为11.7μg/L,最低检出限1.1μg/L,平均批内和批间变异系数分别为5.8%、10.2%;分析不同溶剂对标准曲线和加标回收率的影响,确定PBS 溶液为样本最佳提取溶剂;在玉米、小麦、大米、高粱谷物样本中添加50～500μg/kg 的FB1 标准品,平均回收率在70.5%～105.6% 之间。将该方法应用于40 份谷物样本中FB1 的检测,检测结果与高效液相色谱的相关系数(R2)为0.9547。该方法简单、灵敏、快速、准确,适用于谷物中FB1 的检测。     

直接稀释-超高效液相色谱-串联质谱法快速测定谷物及其制品中16种真菌毒素

目的建立谷物及其制品中黄曲霉毒素、赭曲霉毒素、单端孢霉烯族类毒素、伏马菌素等16种真菌毒素的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。方法 5 g样品加入20 ml乙腈-水-甲酸(79∶20∶1,V/V)溶液提取,10 000 r/min离心5 min后稀释,Cortecs C_(18)色谱柱(100 mm×3.0 mm,1.6μm)分离,以乙腈-0.1%甲酸水作为流动相梯度洗脱,采用四极杆串联质谱仪电喷雾模式检测,同位素稀释内标法定量。结果 16种真菌毒素在线性范围内(0.05~200 ng/ml)具有良好的线性关系,相关系数(r~2)0.99,方法定量限为0.1~50μg/kg,加标回收率为72.67%~126.92%之间,相对标准偏差(RSD)为0.15%~16.83%。应用本方法分析英国弗帕斯检测技术研究所(FAPAS)质控样品,测定结果均在标示范围内,方法准确度良好。结论本方法具有良好的灵敏度、回收率和重复性,前处理方法简单,适用于常规实验室对谷物及其制品中真菌毒素的检测,满足日常真菌毒素监测工作的需要。     

超高压液相色谱法同时检测玉米中的伏马毒素B1、B2、B3

目的 综合比较伏马毒素4种柱前衍生[邻苯二甲醛(OPA)、萘-2,3-二甲醛(NDA)、丹磺酰氯、6-氨基喹啉-N-羟基琥珀酰亚胺氨基甲酸酯(AQC)]效果的优劣, 并选择一种衍生剂用于玉米样品中伏马毒素B1(FB1)、B2(FB2)、B3(FB3)的检测, 建立柱前衍生-超高压液相色谱法同时测定玉米中伏马毒素B1、B2和B3的方法。方法 采用乙腈-水(50∶50, v/v)溶液提取玉米中的伏马毒素B1、B2和B3, 涡旋震荡及离子交换柱净化对玉米样品中的伏马毒素B1、B2和B3进行提取与净化, 经衍生后进行超高压液相色谱-荧光检测器检测。 结果 最终选择OPA衍生作为本研究的衍生方法。3种伏马毒素的线性范围分别为50~1000 ng/mL、25~500 ng/mL、25~500 ng/mL, 相关系数R2均大于0.999; 最低定量限LOQ分别为25.0、14.0、17.0 μg/kg; 3个浓度的加标回收率分别为(75.6?1.6)%~(83.4?2.3)%, (78.9?5.4)%~(90.0?0.7)%, (83.7?8.2)%~(88.6?1.0)%; FB1、FB2和FB3的日间精密度分别为3.62%、3.41%、4.77%。结论 该方法具有预处理简单、检测速度快、灵敏度高的优点, 可满足对玉米中>800 μg/kg伏马毒素含量的检测要求。流动相的改进及梯度洗脱的使用, 提高了检测的灵敏度, 并可被在具有液相色谱仪的实验室应用。     

在线固相萃取-液相色谱-串联质谱法快速测定玉米粉和面粉中伏马毒素

建立在线固相萃取-液相色谱-串联质谱法检测玉米粉和面粉中3种伏马毒素的分析方法。样品用乙腈-水(50∶50,V/V)提取,提取液直接上样,经过WAX在线固相萃取柱净化,以0.1%甲酸溶液和乙腈为流动相,经XBridge C_(18)色谱柱分离,采用电喷雾正电离多反应模式监测,内标法定量。结果表明:伏马毒素B1、伏马毒素B2和伏马毒素B3在0.05~50 ng/m L之间线性关系良好,相关系数均大于0.999 0;检出限和定量限分别为0.08μg/kg和0.2μg/kg;添加水平为0.2~50.0μg/kg时,方法回收率范围为93.9%~117.8%,相对标准偏差范围在1.8%~9.4%。此方法简便快速、灵敏度高,可用于玉米粉和面粉中伏马毒素的准确定量。     

同位素稀释/超高效液相色谱-四极杆-飞行时间质谱法测定牛蛙中50种兽药残留

目的 建立同位素稀释/超高效液相色谱-四极杆-飞行时间质谱法(ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry, UPLC-Q-TOF-MS)测定牛蛙中50种兽药残留的分析方法。方法 样品用0.2%甲酸乙腈提取, 经快速滤过型净化(multi-plug filtration cleanup, m-PFC)固相萃取柱处理, 采用Phenomenex Kinetex C18色谱柱分离, 以0.1%甲酸乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱, 目标物在正离子全信息串联质谱扫描方式(mass spectrometry, MSE)下检测, 内标法定量。结果 50种兽药在各自的质量浓度范围内线性关系良好, 相关系数大于0.995, 检出限为0.5~1.0 μg/kg, 加标回收率为79.4%~112.1%, 相对标准偏差为3.7%~13.1%。结论 该方法前处理简单、结果准确, 适用于牛蛙中50种兽药残留的快速检测。     

乳杆菌脱除伏马毒素的研究

为了探究植物乳杆菌(Lactobacillus plantarum)B7和戊糖乳杆菌(L.pentosus)X8对伏马毒素FB1和FB2脱除作用及影响因素。本文采用高效液相荧光检测的方法研究菌体细胞的伏马毒素脱除率。结果表明植物乳杆菌B7和戊糖乳杆菌X8在37℃吸附1h后对FB1的脱除率分别为52.9%和58.0%,对FB2的脱除率分别达到了85.2%和86.5%。p H、温度、酶影响菌株B7和X8结合伏马毒素FB1和FB2的效果,并且两株菌脱除伏马毒素的作用与其活力无关。两株菌体结合伏马毒素的效率随p H升高而降低。当p H7时,无法检测到两株乳杆菌具有结合伏马毒素的能力。经100℃沸水浴处理后,菌体细胞脱除伏马毒素的效率上升;经溶菌酶处理后,菌体脱除伏马毒素的效率降低。两株乳杆菌具有以吸附方式脱除伏马毒素FB1和FB2的能力,但吸附FB2的效果高于吸附FB1的效果。     

伏马菌素检测技术的研究进展

综述了伏马菌素的危害与各种检测伏马菌素的方法与机理,指出液相色谱-质谱(LC-MS)联合检测和酶联免疫检测是主要的研究方向。。     

Textural Properties of Cold-set Gels Induced from Heat-denatured Whey Protein Isolates

A 9% whey protein (WP) isolate solution at pH 7.0 was heat-denatured at 80°C for 30 min. Size-exclusion HPLC showed that native WP formed soluble aggregates after heat-treatment. Additions of CaCl2 (10–40 mM), NaCl (50–400 mM) or glucono-delta-lactone (GDL, 0.4–2.0%, w/v) or hydrolysis by a protease from Bacillus licheniformis caused gelation of the denatured solution at 45°C. Textural parameters, hardness, adhesiveness, and cohesiveness of the gels so formed changed markedly with concentration of added salts or pH by added GDL. Maximum gel hardness occurred at 200 mM NaCl or pH 4.7. Increasing CaCl2 concentration continuously increased gel hardness. Generally, GDL-induced gels were harder than salt-induced gels, and much harder than the protease-induced gel.     

Occurrence of bisphenol-F-diglycidyl ether (BFDGE) in fish canned in oil

The levels of bisphenol-F-diglycidyl ether (BFDGE) were quantified as part of a European survey on the migration of residues of epoxy resins into oil from canned fish. The contents of BFDGE in cans, lids and fish collected from all 15 Member States of the European Union and Switzerland were analysed in 382 samples. Cans and lids were separately extracted with acetonitrile. The extraction from fish was carried out with hexane followed by re-extraction with acetonitrile. The analysis was performed by reverse phase HPL C with fluorescence detection. BFDGE could be detected in 12% of the fish, 24% of the cans and 18% of the lids. Only 3% of the fish contained BFDGE in concentrations considerably above 1mg/kg. In addition to the presented data, a comparison was made with the levels of BADGE (bisphenol-A-diglycidyl ether)analysed in the same products in the context of a previous study.     

Review of techniques to manufacture micro-hydrogel particles for the food industry and their applications

Microgels are ‘soft’ microscopic cross-linked polymeric particles that are being increasingly exploited in a variety of industries for rheology control, encapsulation and targeted delivery. They are valued because of the ability to tune their functionality to address specific applications in oil recovery, coatings, drug delivery, cosmetics, personal care and foods. Food microgels are typically biopolymer hydrogels in the form of microspheres, nanospheres (also called nanogels), spheroids and fibres. The utilisation of engineered microgels in foods has so far been limited, despite their great potential to address several needs in the food industry, including: satiety control, encapsulation of phytonutrients and prebiotics, texture control for healthier food formulations (e.g. reduced fat products), and targeting delivery to specific areas in the digestive tract. We review the scientific and patent literature on the utilisation and manufacturing methods for producing microgels with an emphasis on micro-hydrogels for food applications.     

12—A CRITIQUE OF SOME HYPOTHESES RELATING TO THE HETEROGENEITY OF THE HIGH-SULPHUR PROTEINS OF WOOL

Joubert and Burns prepared a large number of fractions from the high-sulphur proteins of wool and estimated their molecular weights and amino-acid compositions. Their data have been re-examined in order to look for statistically significant interrelations between amino acids and between the proportion of various amino acids and molecular weight. Statistical analysis of the data is also used to examine the credibility of some hypotheses concerning the mechanism of keratin biosynthesis and to provide further evidence for the existence of families of proteins within the high-sulphur fractions of wool.     

Contribution of European research to risk analysis

The European Commission's, Quality of Life Research Programme, Key Action 1—Health, Food & Nutrition is mission-oriented and aims, amongst other things, at providing a healthy, safe and high-quality food supply leading to reinforced consumer confidence in the safety of European food. Its objectives also include the enhancing of the competitiveness of the European food supply. Key Action 1 is currently supporting a number of different types of European collaborative projects in the area of risk analysis. The objectives of these projects range from the development and validation of prevention strategies including the reduction of consumers risks; development and validation of new modelling approaches; harmonization of risk assessment principles, methodologies, and terminology; standardization of methods and systems used for the safety evaluation of transgenic food; providing of tools for the evaluation of human viral contamination of shellfish and quality control; new methodologies for assessing the potential of unintended effects of genetically modified (genetically modified) foods; development of a risk assessment model for Cryptosporidium parvum related to the food and water industries; to the development of a communication platform for genetically modified organism, producers, retailers, regulatory authorities and consumer groups to improve safety assessment procedures, risk management strategies and risk communication; development and validation of new methods for safety testing of transgenic food; evaluation of the safety and efficacy of iron supplementation in pregnant women; evaluation of the potential cancer-preventing activity of pro- and pre-biotic ('synbiotic') combinations in human volunteers. An overview of these projects is presented here.     

Announcing a new international peer-reviewed journal:Food Science and Human Wellness now accepting manuscript submission in English

<正>We are pleased to announce the launch of a new international peer-reviewed journal-Food Science and Human Wellness,ISSN 2213-4530,which is an open access journal,produced and hosted by Elsevier B.V.on behalf of Beijing Academy of Food Sciences.Food Science and Human Wellness is an international peer-reviewed English journal that provides a forum for the dissemination of     

The Latest Data about Development of Chinese Printing Industry in 2013

In the 2014 China（Shanghai）International Printing Week,Director Wang Yanbin released the latest data about development of Chinese printing industry in 2013.According to statistics,in 2013,the total output value of Chinese printing industry exceeded 1trillion Yuan for the first time,reaching 1.03985 trillion Yuan.There were 105,000 printing enterprises in China,employees were 3.415 million.The total asset was 1.06247 trillion Yuan;     

The State Council Issued "Directory of Government Approved Investment Projects(2013 Edition)"

正On December 2nd,2013,the State Council issued the notification of"Directory of Government Approved Investment Projects(2013 Edition)"(hereafter referred to as"notification").It is pointed out in the"notification"that in order to further deepen reforms in investment systems and administrative examination and approval systems,simplify administrative procedures and delegate powers to lower levels,earnestly     

China textile machinery: taking off in progress

正Among the 1600 exhibitors who take apart in the ITMA ASIA+CITME2014 2/3 are Chinese manufactures.If the numerous figures failed to attract your attention,the increase of quality should draw your focus.To adopt the demand of developing textile machine market,domestic textile machinery enterprises now follow the slogan of"technology drives development"to enhance product competitiveness.Our domestic sellers will showcase product ranging from spinning,weaving,dyeing and printing,     

Top Ten News of China's Paper Industry 2013

On December 24th, 2013, the meeting on the selection of top 10 news of China＇s paper industry 2013 sponsored by 〈China Paper Newsletters〉 was held in Beijing. The yearly selection of the top l0 news, which began in 2000, has become a brand activity widely recognized in the industry thanks to the support from the authorities at all levels and public participation.