超高效液相色谱-串联质谱法测定蔬菜中7种氨基甲酸酯类农药残留

建立蔬菜中氨基甲酸酯类农药残留的超高效液相色谱-串联质谱联用的确证方法。样品经乙腈提取后,氨基柱净化,采用UPLC-MS/MS正离子模式下选择多反应监测(MRM)扫描测定。7种氨基甲酸酯类农药在5～200μg/L范围内线性关系良好,相关系数为0.9977～0.9999。在0.01～0.10mg/kg添加范围内,回收率范围在72.1%～110.2%之间,相对标准偏差为1.7%～9.4%,方法的最低检出限为0.5～8..0μg/kg(RSN=10)。该方法操作简单、灵敏、准确度高,完全可满足蔬菜中多种氨基甲酸酯类农药残留量的测定及确证工作的需要。     

QuEChERS前处理技术与在线凝胶渗透色谱-气相色谱质谱联用法测定蔬菜水果中20种农药残留

目的建立在线凝胶渗透色谱-气相色谱质谱(online gel permeation chromatography-gas chromatography/mass spectrometry,GPC-GC/MS)联用法测定蔬菜、水果中有机磷、氨基甲酸酯、拟除虫菊酯类20种农药残留的分析方法。方法蔬菜、水果中有机磷、氨基甲酸酯、拟除虫菊酯类20种农药残留经过乙腈与Qu ECh ERS试剂包提取、净化、浓缩,经在线凝胶渗透色谱-气相色谱质谱仪分析测定,选择离子模式定量。结果 GPC-GC/MS系统中的GPC弥补了Qu ECh ERS方法净化干扰物质不彻底的问题,从而降低分析背景,改善峰形,提高分析结果的准确性和相关质谱图匹配性。在0.01 mg/kg加标情况下,3种样品(芹菜、桔子和韭菜)除桔子和韭菜中甲胺磷、敌敌畏和氧化乐果由于基质的影响而回收率偏低外,其他均在80%~120%,3种样品平行样的相对标准偏差均在15%以下,并且该方法与传统的固相萃取小柱净化法进行加标比对,回收率无明显差异。结论 Qu ECh ERS方法和GPC-GC/MS联合使用分析蔬菜水果中的农药残留,达到了快速、简单、便宜、有效、可靠和安全的目的。     

UPLC-MS/MS测定蔬菜中氨基甲酸酯类农药

建立超高效液相色谱-串联质谱(UPLC-MS/MS)测定蔬菜中氨基甲酸酯类农药的方法。用乙腈提取蔬菜中的氨基甲酸酯类农药,经QuEChERS净化后UPLC-MS/MS定量分析。实验浓度范围内线性关系良好,方法加标回收率在82.2%~104.1%,精密度(RSD)为1.9%~4.0%,检出限为0.2~1.5μg/kg。UPLC-MS/MS法测定蔬菜中氨基甲酸酯类农药有较好的回收率、重现性和较低的检出限,能满足大批量样品氨基甲酸酯类农药的快速检测需求。     

气相色谱-串联质谱结合QuEChERS方法检测蔬菜、水果中37种农药残留

本文旨在探究气相色谱-串联质谱结合QuEChERS方法检测蔬菜、水果中37种农药残留的效果。方法:对选取的蔬菜水果进行取样和提取,采用气相色谱-串联质谱结合QuEChERS方法进行农药残留检测。结果:130份样品中有4份为阳性,样品中农药残留率为3.08%。对检测结果为阳性的样品利用GB/T19648-2006的标准程序和方法,进行GC-MS/MS法进行重新检测,结果与本研究所用方法检测结果一致,且农药残留量基本相当。结论:气相色谱-串联质谱结合QuEChERS方法在检测蔬菜、水果的农药残留上具有较高的准确性,同时还具有快速、灵敏的优点。     

全自动固相萃取-气相色谱-三重四级杆质谱法检测蔬菜中23种农药残留

目的建立蔬菜中有机磷类、拟除虫菊酯类共23种农药残留的分析方法。方法样品加丙酮-二氯甲烷(1∶1,V/V)混合溶剂提取后经全自动固相萃取仪净化,采用气相色谱-三重四级杆串联质谱的多反应监测模式进行检测,内标法定量。结果 23种农药在0.05~0.80 mg/L范围内线性良好,相关系数均大于0.993 3;加标回收率在75.0%~105.5%之间;方法的检出限为0.02~0.70 mg/kg。在少量蔬菜样品中发现氯氰菊酯和氯氟氰菊酯超标。结论该方法适用于蔬菜中多种农药残留的快速筛查测定。     

多壁碳纳米管分散固相萃取净化-气相色谱三重四级杆质谱联用同时测定桂皮中10种有机磷农药

建立一种多壁碳纳米管分散固相萃取净化-气相色谱三重四级杆质谱联用同时测定桂皮中10种有机磷农药的检测方法。样品经乙腈提取,以MWCNTs、PSA和MgSO_4净化,离心、过滤后经气相色谱三重四级杆质谱测定,外标法定量。结果表明,10种有机磷农药在0.01~1.0μg/mL范围内具有良好的线性。加标回收率为78.3%~105.2%,相对标准偏差(n=5)为1.6%~9.2%,方法检出限为0.001~0.010mg/kg。该方法操作简单快捷、准确、检测成本低,能满足桂皮中有机磷农药残留的检测要求。     

溶剂吸收-气相色谱-质谱法测定食用菌中二硫代氨基甲酸酯类农药

目的建立食用菌中二硫代氨基甲酸酯类农药残留的溶剂吸收-气相色谱-质谱测定方法。方法样品在氯化亚锡盐酸溶液中加热发生消化反应,生成二硫化碳,冷却后用正己烷萃取出二硫化碳,经Hp-VOC色谱柱(60 m×0.20 mm,1.12μm)分离,选择离子监测(SIM)模式气相色谱-质谱进行检测,外标标准曲线法定量。结果食用菌中添加0.025、0.05、0.25 mg/kg 3个水平的标准溶液,回收率的范围为94.8%～109%,相对标准偏差为3.7%～5.5%(n=3)。检出限为0.01 mg/kg,定量限为0.02 mg/kg。结论该方法具有操作简单、准确度高和精密度好等优点,可适用于食用菌中二硫代氨基甲酸酯类农药残留的测定。     

在线凝胶渗透色谱-气相色谱质谱联用仪测定药食同源样品中30种农药残留

目的建立药食同源食品中多种农药残留检测的在线凝胶渗透色谱-气相色谱-质谱联用法(gel permeation chromatography-gas chromatography-mass spectrometry, GPC-GC-MS)。方法本研究采用3种不同净化方式对药食同源样品进行前处理,利用在线凝胶渗透色谱-气相色谱质谱联用仪测定样品中30种农药残留。结果结果表明30种农药在0.01～0.2μg/mL浓度范围内线性关系良好,检出限为0.01 mg/kg,药食同源样品3个水平添加回收为69.1%～88.8%,相对标准偏差为3.3%～19.4%。结论3种方法中QuEChERS法灵敏度高,准确性好,可用于药食同源样品中多种农药残留的同时测定。     

大气压气相色谱电离源-串联质谱法测定蔬菜中23种农药残留

目的 建立蔬菜中23种农药的大气压气相色谱电离源-串联质谱检测方法。方法 采用丙酮提取蔬菜样品中的目标农药,多壁碳纳米管为净化材料,经DB-5MS色谱柱(30 m×0.25 mm,0.25 μm)分离,结合大气压气相色谱电离源技术,正离子多反应监测(MRM)模式进行检测,外标标准曲线法定量。结果 23种农药在0.01～20 μg/L范围内线性良好,相关系数(R²)均大于0.99,在蔬菜基质中23种农药的方法检出限和定量限分别为0.02～0.40和0.05～1.25 μg/kg,回收率为66.7%～110.7%,相对标准偏差(RSD)≤14.8%。结论 本方法具有良好的灵敏度、重现性和特异性,适用于蔬菜中多种农药残留的快速检测。     

基于GC-MS/MS技术对承德地区山楂中44种农药残留分析评价

目的：对承德地区山楂中44种农药残留进行检测分析并评价。方法：利用气相色谱-质谱/质谱联用方法检测山楂样品中44种农药残留含量。结果：44种农药残留组分在0.2～0.6μg·mL^-1线性关系良好,相关系数均大于0.998,加标回收率在70.8%～104.5%,相对标准偏差在0.18%～5.20%。结论：承德地区山楂产品安全性较高,病虫害综合防治技术较好,能够为食品安全监管提供数据支持。     

Reliable identification of grapevine rootstock varieties using RAPD PCR on woody samples

Since grapevine ( Vitis spp .) rootstock material is being traded increasingly as disbudded woody material a lack of distinctive morphological features on such material necessitates an alternative and reliable means of identification. Methods described here were developed for rapid and efficient extraction of DNA from woody samples rich in phenolic compounds and polysaccharides, and for subsequent identification of varieties by RAPD PCR. Using these methods, and with the application of only one selected RAPD primer, we were able to differentiate sixteen rootstock varieties, including the seven varieties most commonly used in Germany. Problems commonly encountered with reproducibility of RAPD patterns were avoided by choosing primers with a dinucleotide sequence and a high G/C content that allowed a rather high annealing temperature of 45°C. Methods described here should also be useful for other horticultural crops, especially those with woody tissues rich in phenolic compounds and polysaccharides.     

Aroma characterization of various apricot varieties using headspace–solid phase microextraction combined with gas chromatography–mass spectrometry and gas chromatography–olfactometry

The characterization of the aromatic profile of several apricot cultivars with molecular tracers in order to obtain objective data concerning the aromatic quality of this fruit was undertaken using headspace–solid phase microextraction (HS–SPME). Six apricot cultivars were selected according to their organoleptic characteristics: Iranien, Orangered, Goldrich, Hargrand, Rouge du Roussillon and A4025. The aromatic intensity of these varieties measured by HS–SPME–Olfactometry were defined and classified according to the presence and the intensity of grassy, fruity and apricot like notes. In the six varieties, 23 common volatile compounds were identified by HS–SPME–GC–MS. Finally, 10 compounds, ethyl acetate, hexyl acetate, limonene, β-cyclocitral, γ-decalactone, 6-methyl-5-hepten-2-one, linalool, β-ionone, menthone and (E)-hexen-2-al were recognized by HS–SPME–GC–O as responsible of the aromatic notes involved in apricot aroma and considered as molecular tracers of apricot aromatic quality which could be utilized to discriminate apricot varieties.     

Tests of potential functional barriers for laminated multilayer food packages. Part I: Low molecular weight permeants

The advent of the functional barrier concept in food packaging has brought with it a requirement for fast tests of permeation through potential barrier materials. In such tests it would be convenient for both foodstuffs and materials below the functional barrier (sub-barrier materials) to be represented by standard simulants. By means of inverse gas chromatography, liquid paraffin spiked with appropriate permeants was considered as a potential simulant of sub-barrier materials based on polypropylene (PP) or similar polyolefins. Experiments were performed to characterize the kinetics of the permeation of low molecular weight model permeants (octene, toluene and isopropanol) from liquid paraffin, through a surrogate potential functional barrier (25 μm-thick oriented PP) into the food simulants olive oil and 3% (w/v) acetic acid. These permeation results were interpreted in terms of three permeation kinetic models regarding the solubility of a particular model permeant in the post-barrier medium (i.e. the food simulant). The results obtained justify the development and evaluation of liquid sub-barrier simulants that would allow flexible yet rigorous testing of new laminated multilayer packaging materials.     

Analysis of benzo[a]pyrene in spiked fatty foods by second derivative synchronous spectrofluorimetry after microwave-assisted treatment of samples

A simple, rapid and inexpensive method has been developed for the determination of benzo[a     

The development of reference materials for paralytic shellfish poisoning toxins in lyophilized mussel. II: Certification study

This paper describes the second part of a project undertaken to develop certified mussel reference materials for paralytic shellfish poisoning toxins. In the first part two interlaboratory studies were undertaken to investigate the performance of the analytical methodology for several PSP toxins, in particular saxitoxin and decarbamoyl-saxitoxin in lyophilized mussels, and to set criteria for the acceptance of results to be applied during the certification exercise. Fifteen laboratories participated in this certification study and were asked to measure saxitoxin and decarbamoyl-saxitoxin in rehydrated lyophilized mussel material and in a saxitoxin-enriched mussel material. The participants were allowed to use a method of their choice but with an extraction procedure to be strictly followed. The study included extra experiments to verify the detection limits for both saxitoxin and decarbamoyl-saxitoxin. Most participants (13 of 15) were able to meet all the criteria set for the certification study. Results for saxitoxin.2HCl yielded a certified mass fraction of <0.07 mg/kg in the rehydrated lyophilized mussels. Results obtained for decarbamoyl-saxitoxin.2HCl yielded a certified mass fraction of 1.59+/-0.20 mg/kg. The results for saxitoxin.2HCl in enriched blank mussel yielded a certified mass fraction of 0.48 +/- 0.06 mg/kg. These certified reference materials for paralytic shellfish poisoning toxins in lyophilized mussel material are the first available for laboratories to test their method for accuracy and performance.     

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     

Chinese CTP Market

According to Printing and Printing Equipment Industries Association of China（PEIAC）＇s statistics to the plate manufucturer in China, in 2013, the actual offset plate production has reached 346 million square meters in China. Among them, the CTP production volume was 245 million square meters, up by 11% than that of last year; the total sales of the CTP plate was 239 million square meters, up by 13%.     

Preparatory Work of Print China 2015 is Going Smoothly

正Held at Guangdong Modern International Exhibition Center,Print China 2015 will cover 7exhibition halls,besides the original Hall No.3,4,5,6,7,the newly built F zone of Hall 3 will be used too.The total area will be140,000 square meters.Hall 3:Offset and large printing equipment,package printing equipment,post press     

INFOPRINT 2014 was Successfully Held in Dongguan

Sponsored by Printing and Printing Equipment Industries Association of China （PEIAC） and organized by Print China magazine, the Seventeenth Beijing International Printing Information Conference （INFOPRINT 2014） was successfully held on 11th Dec. 2014 at Dongguan Exhibition International Hotel.