QuEChERS-超高效液相色谱-串联质谱法同时测定畜禽肉中11 种喹诺酮类兽药残留

建立一种超高效液相色谱-串联质谱法测定畜禽肉中恩诺沙星、环丙沙星、氧氟沙星、培氟沙星、诺氟沙星、洛美沙星、沙拉沙星、双氟沙星、司帕沙星、氟罗沙星和达氟沙星共11 种喹诺酮类兽药残留的检测方法。畜禽肉样品经2%甲酸-乙腈均质提取,离心沉淀后上清液经QuEChERS净化剂净化后,经快速溶剂蒸发系统浓缩,采用Waters BEH C18色谱柱（2.1 mm×50 mm,1.7 μm）分离,以0.1%甲酸-水和0.1%甲酸-乙腈为流动相进行梯度洗脱,电喷雾离子源电离,多反应监测模式采集信号,内标法定量。结果表明：11 种喹诺酮类兽药在2～80 ng/mL质量浓度范围内线性关系良好（R2＞0.99）,方法的检出限和定量限分别为0.5～2.0 μg/kg和1.5～6.0 μg/kg;空白样品加标量为10、25、50 μg/kg 3 个水平时,11 种喹诺酮类兽药的平均加标回收率为74.52%～106.83%,相对标准偏差为1.8%～8.7%（n=6）。该方法检测过程简单快捷、准确度好、灵敏度高,适用于畜禽肉中喹诺酮类兽药残留的检测。     

HPLC-MS/MS法快速测定乳制品中90种兽药的残留量

目的 建立高效液相色谱-串联质谱法（HPLC-MS/MS）测定乳制品中十大类90种兽药残留的检测方法。方法 试样用0.2%甲酸乙腈溶液提取,经Waters Prime HLB固相萃取柱净化,用Waters XBridge BEH-C18色谱柱洗脱分离,并使用电喷雾电离源,正负离子切换扫描模式进行检测,外标法定量。结果90种兽药在1 ng/mL～20 ng/mL范围内呈现良好的线性相关性,相关系数均大于0.995。90种兽药的方法检出限为0.3 ?g/kg,方法定量限为1 ?g/kg。在添加量为1 ?g/kg、2 ?g/kg和10 ?g/kg的加标回收实验下,90种兽药的加标回收率范围分别为66.0%～134.8%,64.0%～122.4%和62.4%～118.3%。同时做了方法精密度验证,有69%的兽药RSD<5%,有28%的兽药RSD在5%～10%,有3%的兽药RSD在10%～20%。结论 该方法简单、快速、高效且能同时准确定性和定量检测乳制品中十大类90种兽药的残留量。     

超高效液相色谱-串联质谱法测定牛乳中6种兽药残留

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）测定牛奶样品中6种兽药残留（硝碘酚腈、碘醚柳胺、氯氰碘柳胺、托曲珠利、三氯苯达唑、水杨酸钠）的检测方法。方法:样品经过乙腈溶液提取,以MAX固相萃取柱净化,采用Waters X Bridge BEH-C₁₈色谱柱分离,流动相以乙腈和0.1%甲酸水溶液梯度洗脱,并使用电喷雾离子源,正负离子切换扫描模式进行检测,外标法定量。结果:6种兽药在0~10 ng/mL范围内呈现良好的线性关系,决定系数（R2）均大于0.995。6种兽药方法的检出限为0.06~0.18 μg/kg,方法的定量限为0.5~2.0 μg/kg。在添加量为0.5~8.0 μg/kg的加标回收实验下,6种兽药加标回收率为67.1%~105.5%,相对标准偏差均小于10%。结论:该方法前处理操作简便,分析速度快,灵敏度高,可用于牛奶样品中的兽药残留测定。     

固相萃取结合超高效液相色谱-质谱法测定畜禽肉及肉制品中肾上腺素和多巴胺的残留量

建立畜禽肉及肉制品中2 种儿茶酚胺类化合物（肾上腺素和多巴胺）的超高效液相色谱-质谱联用检测方法。样品采用10 mmol/L磷酸二氢钾溶液提取,WCX固相萃取柱净化,Waters Acquity BEH C18柱分离,采用电喷雾离子源,正离子多反应模式监测,基质匹配内标法定量。结果表明：肾上腺素和多巴胺在0.5～50 ng/mL范围内,相关系数（R2）均大于0.996;在畜肉中的检出限和定量限分别为0.39～0.40 μg/kg和1.00 μg/kg,在禽肉中的检出限和定量限分别为0.36～0.37 μg/kg和0.98 μg/kg,在肉制品中的检出限和定量限分别为0.38 μg/kg和0.96～0.97 μg/kg;加标量为1～10 μg/kg时,方法回收率为83.7%～111.2%,相对标准偏差为1.28%～5.76%。该方法具有灵敏度高、定量准确等优点,适用于畜禽肉及肉制品中残留儿茶酚胺类化合物含量的测定。     

超高效液相色谱-串联质谱法同时测定鸡肉中43种兽药残留

目的建立正负离子切换-超高效液相色谱-串联质谱法同时测定鸡肉中43种兽药残留量的分析方法。方法鸡肉样品经甲酸提取液涡旋提取,固相萃取净化, 10 mmol/L甲酸铵稀释, ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm, 1.8μm)色谱柱分离,以0.05%甲酸溶液和0.05%乙腈进行梯度洗脱,正离子多反应监测39种兽药,负离子多反应检测4种兽药,外标法定量测定药物的含量。结果 43种兽药定量限为5μg/kg,标准曲线在0.4～100.0 ng/mL范围内均呈良好的线性关系。在空白鸡肉中3个不同添加水平下,平均回收率为60%～120%之间,变异系数为0.7%～12%。结论该方法准确、快速、灵敏、稳定,适合作为鸡肉中43种兽药残留量的测定。     

固相萃取-超高效液相色谱-串联质谱法同时测定禽蛋中12种禁用兽药残留

目的 建立一种超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)正负同时扫描检测禽蛋中12种禁用兽药残留的方法。方法 样品经1.0%甲酸乙腈提取,经 PRiME HLB （PRiME Hydrophilic-Lipophilic Balance,PRiME HLB ）固相萃取柱净化,氮气浓缩至干后,残渣用流动相溶解, 目标物用ACQUITY UPLC?HSS T3色谱柱（50 mm×2.1 mm,1.8 μm）分离,以乙腈和0.02%甲酸+5 mmol/L乙酸铵水溶液为流动相进行梯度洗脱,用UPLC-MS/MS法进行检测,内标法定量。 结果 12种兽药在 0. 50μg / L ~ 300μg / L 浓度范围内线性良好,相关系数均大于0.99,检出限在0.05 ~1.5 μg/kg之间,定量限在0.10 ~3.0 μg/kg之间。加标回收率为80.0%～114.2%,相对标准偏差为2.09%～10.2%,结论 该方法前处理简单、准确、成本较低,适用于禽蛋中兽药残留的高通量快速检测分析。     

PRiME HLB固相萃取-高效液相色谱-串联质谱法同时快速测定鸡蛋中48种兽药残留

建立固相萃取-高效液相色谱-串联质谱同时快速测定鸡蛋中48种兽药残留的分析方法。样品采用90%乙腈水溶液提取,用PRiME HLB小柱净化浓缩后用电喷雾离子源,正负离子扫描,多反应监测模式的高效液相色谱-串联质谱法进行检测,以基质匹配曲线外标法定量。正离子采用CAPCELL PAK C18 MGⅢ-H色谱柱,流动相为0.05%甲酸乙腈和0.1%甲酸水;负离子采用ACQUITY UPLC BEH C18色谱柱,流动相为5 mmol/L乙酸铵和乙腈。结果表明,鸡蛋样品中的48种兽药残留在0.5~50 μg/kg浓度范围内线性关系良好,相关系数(r)为0.9952~1.0000。方法检出限为0.01~0.55 μg/kg,定量限为0.03~1.83 μg/kg,样品回收率在63.3%~111.4%之间,相对标准偏差小于10%(n=3)。本方法操作快速简单,重复性好,灵敏度较高,适用于鸡蛋中48种兽药残留的快速筛查检测。     

快速高分离液相色谱- 串联质谱法对肌肉组织中糖皮质激素残留的检测

建立采用快速高分离液相色谱- 串联质谱(UHPLC-MS2)技术检测肌肉组织中糖皮质激素残留的方法。样品经乙酸乙酯提取,固相萃取法净化,以C18 色谱柱(150mm × 2.1mm,3.5μm)为分离柱,水- 乙腈- 甲酸溶液为流动相进行梯度洗脱,快速高分离液相色谱- 串联质谱ESI 负离子模式进行检测。该方法线性范围为0.5～5ng/mL,线性相关系数R2 ≥ 0.9963,检测限：倍氯米松为1.0μg/kg,氢化可的松为2.0μg/kg,其余均为0.5μg/kg。平均回收率为82.75%～91.87%,相对标准偏差≤ 4.43%(n=5)。     

高效液相色谱-串联质谱法测定卤肉中3种β-受体激动剂残留

建立卤肉中3种β-受体激动剂(克仑特罗、莱克多巴胺、沙丁胺醇)残留检测的高效液相色谱-串联质谱方法。样品经β-盐酸葡萄糖醛甙酶/芳基硫酯酶水解,MCX固相萃取柱净化,以乙腈-0.1%甲酸溶液作为流动相洗脱,采用电喷雾离子源,多反应监测方式进行采集,外标法定量。结果表明：3种β-受体激动剂在1～100ng/mL质量浓度范围内呈现良好的线性关系,R2均大于0.99,方法检测限均为0.25μg/kg,从0.5、1μg/kg和2μg/kg添加水平检测结果可以看出,方法平均回收率为80%～120%,相对标准偏差为1.0%～10.0%。     

超高效液相色谱-串联质谱法检测牛组织中常山酮残留量

为了建立牛组织中常山酮残留量的超高效液相色谱-串联质谱检测方法,将牛组织中的常山酮经蛋白酶酶解后,采用乙酸乙酯提取,HLB固相萃取柱净化,超高效液相色谱-串联质谱法进行检测。在0.5 ng/mL～50 ng/mL线性范围内,常山酮的回归方程呈良好的线性关系,R2＞0.998,牛组织样品在添加水平为0.5、5 μg/kg时,回收率为73.2%～93.60%,相对标准偏差（relative standard deviation,RSD）为 5.91%～7.96%,方法检出限为 0.25 μg/kg,定量限为 0.5 μg/kg。本试验适用于牛组织中常山酮残留量的检测。     

An internet compendium of analytical methods and spectroscopic information for monomers and additives used in food packaging plastics

An internet website (http://cpf.jrc.it/smt/) has been produced as a means of dissemination of methods of analysis and supporting spectroscopic information on monomers and additives used for food contact materials (principally packaging). The site which is aimed primarily at assisting food control laboratories in the European Union contains analytical information on monomers, starting substances and additives used in the manufacture of plastics materials. A searchable index is provided giving PM and CAS numbers for each of 255 substances. For each substance a data sheet gives regulatory information, chemical structures, physico-chemical information and background information on the use of the substance in particular plastics, and the food packaging applications. For monomers and starting substances (155 compounds) the infra-red and mass spectra are provided, and for additives (100 compounds); additionally proton NMR are available for about 50% of the entries. Where analytical methods have been developed for determining these substances as residual amounts in plastics or as trace amounts in food simulants these methods are also on the website. All information is provided in portable document file (PDF) format which means that high quality copies can be readily printed, using freely available Adobe Acrobat Reader software. The website will in future be maintained and up-dated by the European Commission's Joint Research Centre (JRC) as new substances are authorized for use by the European Commission (DG-ENTR formerly DGIII). Where analytical laboratories (food control or other) require reference substances these can be obtained free-ofcharge from a reference collection housed at the JRC and maintained in conjunction with this website compendium.     

Detection of adulteration of locust bean gum with guar gum by capillary electrophoresis and polarized light microscopy

Capillary electrophoresis (CE) and polarized light microscopy (PLM) were utilized in the detection of the adulteration of locust bean gum with guar gum. For CE analyses, standards of locust bean and guar gums were extracted with 30% CH₃CN, removing the residual proteins from the gum matrix. A 8.75 mM NaH₂PO₄-20.6 mM Na₂B₄O₇ buffer, pH 9, was used to separate these proteins and to identify marker proteins that were present in the guar gum. These markers did not co-migrate with components in the extracts of mechanically processed locust bean gum, and are used as indicators of adulteration. Using PLM with toluidine blue and iodine staining techniques, unadulterated locust bean gum samples were distinguished from mixed samples through the differential staining of components in locust bean versus guar and tara gums. These experiments in the use of CE and PLM provide orthogonal and complementary methods for the verification of 'true' positives and the elimination of 'false' positives.     

10—THE WRINKLING BEHAVIOUR OF WOOL FABRICS: THE EFFECT OF ANNEALING AND CROSS-LINKING

An investigation is described in which various polyfunctional compounds were applied to wool in attempts to stabilize the temporary improvements in wrinkle-recovery brought about by ‘annealing’. Several reactive systems involving formaldehyde were found to produce the desired permanently improved wrinkle-recovery.     

"National Strategy on Adaptation to Climate Changes" Issued

On November 18th, 2013, the ＂National Strategy on Adaptation to Climate Changes＂ （hereafter referred to as the ＂The Strategy＂ ） jointly formulated by Nationa Development and Reform Commission, Ministry of Finance Ministry of Housing and Urban-Rural Development Ministry of Transport, Ministry of Water Resources, Ministry of Agriculture, Bureau of Forestry, China Meteorologica Administration, and State Oceanic Administration was issued by the agencies with an announcement on the issuance.     

Ministry of Industry and Information Technology Confirmed 2014 Main Expected Targets for Energy-Saving and Comprehensive Utilization

Ministr y of Industr y and Information Technology confirmed that the main expected targets for energysaving and comprehensive utilization in 2014 are：energy consumption and CO2 emissions per unit of industrial added-value decreases by 4.5%,water consumption per ten thousand Yuan of industrial added-value decreases by7%,comprehensive utilization of industrial solid waste is further improved,and pollution emissions in key industries is markedly reduced.     

2013 Annual Report of China's Paper Industry

According to the survey made by China Paper Association （CPA）, in 2013, there were about 3,400 paper ＆ board manufacturers. The total production and consumption of paper ＆ board were 101.10 million tons and 97.82 million tons, decreased by 1.37% and 2.65% compared to the previous year respectively; paper ＆ board per capita consumption was 72 kg. From 2004 to 2013, the average annual growth rate of paper ＆ board production was 8.26%, and the average annual growth rate of paper ＆ board consumption was 6.74%. As shown in Fig. 1.     

2014 China International Paper Technology Exhibition and Conference （CIPTE） Will Be Held in Shanghai

In order to promote the development of China＇s paper industry, display the technical achievements of a conlmu of paper nication paper industry, and provide platform for the enterprises and relative industries, China Paper Association,     

Excellent Enterprises:keep on leading technology

正As a biennial industry event,ITMA ASIA+CITME2014 has attracted leading enterprises within global textile industry from Europe,American and Japan etc..To showcase the comprehensive development of oversea enterprises,The Textile Machiney Magazine has selected representative enterprises ranging from spinning,weaving,chemical fiber,knitting,nonwovensindustrial,accessories,dyeing and printing,to exhibit their advanced technology and equipment.In the era that global textile industry have ushered a new round     

Distribution and stability of aflatoxin M1 during processing, ripening and storage of Telemes cheese

Telemes cheeses were produced using milk that was artificially-contaminated with aflatoxin M1 at the levels of 0.050 and 0.100 microg/l. The cheeses produced in the two cheese-making trials were allowed to ripen for 2 months and stored for an additional 4 months to simulate commercial production of Telemes cheese. Concentrations of aflatoxin M1 in whey, curd, brine, and the produced cheeses were determined at intervals by liquid chromatography and fluorometric detection coupled with immunoaffinity column extraction. Concentrations of aflatoxin M1 in the produced curds were found to be 3.9 and 4.4 times higher than those in milk, whereas concentrations in whey were lower than those in curd and milk. Aflatoxin M1 was present in cheese at higher concentrations at the beginning than at the end of the ripening/storage period, and it declined to concentrations 2.7 and 3.4 times higher than those initially present in milk by the end of the sixth month of storage. Concentrations of aflatoxin M1 in brine started low and increased by the end of the ripening/storage period but only a portion of the amounts of aflatoxin M1 lost from cheese was found in the brine. Results showed that Telemes cheeses produced from milk containing aflatoxin M1 at a concentration close to either the maximum acceptable level of 0.05 microg/l set by the European union (EU) or at double this value, will contain the toxin at a level that is much lower or slightly higher, respectively, than the maximum acceptable level of 0.250 microg of aflatoxin M1/kg cheese set by some countries.     

Analysis of plasticizers in cap-sealing resins for bottled foods

A survey of plasticizers in cap-sealing resins for bottled foods has been undertaken. During 1997-1999 di-(2- ethylhexyl)phthalate (DEHP) was found in seven out of 21 samples on the Japanese domestic market and in 10 out of 61 imported samples as well as a further two samples which contained di-(2-ethylhexyl)adipate (DEHA). In the period 1993-1999, of the other plasticizers diacetyl lauroyl glycerol (DALG) was only detected in domestic samples whereas diisodecyl phthalate (DIDP) and diisononyl phthalate (DINP) were only in imported samples. It was observed overall that DEHP and DEHA were restricted to use in cap-sealing resins for bottled foods. Whilst phthalates, DEHA or DALG were detected in samples in 1993 and 1995, the investigation in 1997-1999 showed fewer samples in which these plasticizers were found.