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1.
目的:建立超高效液相色谱-串联质谱法测定调味料中吗啡、可待因、蒂巴因、那可丁和罂粟碱残留量的分析方法。方法:样品用水分散、乙腈超声提取,经盐析、低温高速离心分层后,样液于40℃水浴氮吹近干,用10%乙腈溶液(含0.1%甲酸)溶解残渣,再经低温高速离心、过膜上机测定;以Kinetex? 2.6μm Biphenyl 100?色谱柱(100 mm×3.0 mm)分离,0.1%甲酸-水和0.1%甲酸-甲醇为流动相进行梯度洗脱,电喷雾电离(ESI),正离子模式,多反应监测(MRM)下检测,吗啡、可待因用内标法定量,蒂巴因、那可丁、罂粟碱用外标法定量。结果:吗啡、可待因在0.5~20.0 ng/mL,蒂巴因在0.10~4.0 ng/mL,那可丁、罂粟碱在0.05~2.0 ng/mL范围内均有良好的线性关系,相关系数r均大于0.998。吗啡、可待因的方法检出限为1.0μg/kg,蒂巴因的方法检出限为0.2μg/kg,那可丁、罂粟碱的方法检出限为0.1μg/kg。5种生物碱的加标回收率在75.2%~117.3%之间,相对标准偏差均小于15%。结论:该方法操作简单,具有较高的灵敏...  相似文献   

2.
目的建立检测火锅调料中非法添加罂粟壳(粉)的方法。方法样品经QuEChERS方法提取、净化后,采用超高效液相色谱串联三重四极杆质谱仪(UPLC-MS),在多反应监测(MRM)模式下,通过色谱、质谱条件优化及方法学考察,建立了高效、准确检测火锅调料中非法添加罂粟壳(粉)的方法。结果本方法的线性范围为:那可丁2.470~49.405ng/mL,r=0.9994;罂粟碱2.090~41.804 ng/mL,r=0.9995;蒂巴因2.042~40.840 ng/mL,r=1.000;可待因11.287~225.733ng/mL,r=0.9996;吗啡10.420~208.400 ng/mL,r=0.9999。那可丁、罂粟碱、蒂巴因、可待因、吗啡的检测限分别为0.21,0.33,0.31,10.37,4.11μg/kg。回收率78.4%~100.6%。结论本方法快速、准确、灵敏度高,可用于检测火锅调料中的罂粟壳(粉)。  相似文献   

3.
针对市售餐饮小龙虾,利用QuEChERS方法进行前处理,建立超高效液相色谱-串联质谱(UPLCMS/MS)联用法检测小龙虾中吗啡、可待因、那可丁、罂粟碱、蒂巴因5种生物碱的分析方法。样品经粉碎搅匀制备后用0.1 mol/L盐酸溶液涡旋分散并超声处理30 min,然后利用乙腈及QuEChERS粉末(6 g无水硫酸镁与1.5 g无水醋酸钠)提取,离心后吸取上清溶液进样分析。色谱分离条件为:固定相采用ACQUITY UPLCTM BEH HILIC色谱柱(1.7μm,2.1×100 mm),流动相采用分别含0.1%甲酸的乙腈和0.1%甲酸的10 mmol/L甲酸铵溶液进行梯度洗脱,经电喷雾正离子(ESI+)模式电离及多反应监测(MRM)分析和定量测定目标化合物,并选用9种市售小龙虾作为试样进行检验。结果表明,内标法定量分析吗啡、可待因的线性浓度范围为5~250 ng/mL,外标法定量分析罂粟碱、那可丁、蒂巴因的线性浓度范围为1~50 ng/mL,在线性范围内峰面积与进样浓度(ng/mL)间的相关系数均大于0.995。5种生物碱的检出限为0.6~3.7μg/kg,定量限为...  相似文献   

4.
研究建立火锅底料中非法添加罂粟壳的液相色谱-串联质谱测定法。采用水提取,乙腈和无水醋酸钠萃取罂粟壳中的生物碱分,液质联用进行检测,采用色谱柱SHISEIDO CAPCELL PAK CR1∶4(5μm,2.0×150 mm)色谱分离,流动相为乙酸铵:乙腈(50∶50),0.5%甲酸为A相,乙腈为流动相B相。该方法的检出限为1 ng/mL,方法定量下限吗啡为37μg/kg,可待因、罂粟碱、蒂巴因和那可丁为1μg/kg,线性范围为1 ng/m~40 ng/mL,加标回收率64.2%~101.1%。该方法测定火锅底料罂粟碱中吗啡、可待因、罂粟碱、那可丁、蒂巴因5种生物碱的含量快速、准确,适合于火锅调味料食品中罂粟壳的检测。  相似文献   

5.
目的:研究探讨基质效应、标曲定量方式对餐饮食品中5种生物碱定量结果的影响,建立一种高效Qu ECh ERS-UPLC-MS/MS方法,一次性同时检测羊汤、火锅汤和水煮鱼汤3种餐饮食品中罂粟碱、那可丁、蒂巴因、吗啡、可待因5种生物碱的含量。方法:试样经高效Qu ECh ERS前处理提取净化,通过UPLCMS/MS正离子MRM模式进行测定。结果:罂粟碱、那可丁、蒂巴因在羊汤、火锅汤和水煮鱼汤3种餐饮食品中表现为弱的基质效应抑制,吗啡、可待因表现为中等基质效应抑制;高效Qu ECh ERS前处理可以满足罂粟碱、那可丁、蒂巴因的提取效率要求,而不能满足吗啡、可待因的提取效率要求,需要采用内标物质进行校正。采用溶剂标曲外标法定量分析罂粟碱、那可丁、蒂巴因和溶剂标曲内标法定量分析吗啡、可待因,罂粟碱、那可丁、蒂巴因线性范围为0.20~5.00 ng·mL-1,吗啡、可待因线性范围为1.00~25.00 ng·mL-1,相关系数均在0.998以上,方法检出限位于0.02~1.35μg·kg-1,加标回收率控制在69%~88%,相对标准...  相似文献   

6.
建立改进的QuEChERS(quick, easy, cheap, effective, rugged, safe)方法,以内标法结合超高效液相色谱-串联质谱法(ultra high performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定肉制餐饮食品中吗啡、可待因、那可丁、罂粟碱、蒂巴因5 种罂粟壳生物碱。样品经乙腈-体积分数0.1%氨水提取,净化包(2 g无水硫酸镁、50 mg N-丙基乙二胺,100 mg C18E)净化,选择含10 mmol/L甲酸铵的体积分数0.1%甲酸-水溶液和体积分数0.1%甲酸-乙腈溶液作为流动相,采用等度洗脱,使净化液中5 种罂粟壳生物碱经HILIC Core-shell色谱柱(50.0 mm×2.1 mm,1.7 μm)分离,在多反应监测模式下利用电喷雾电离源正离子模式扫描获得质谱数据,内标法定量。结果表明:5 种罂粟壳生物碱可在8 min内有效分离,且罂粟碱、那可丁、蒂巴因在0.2~20.0 ng/mL质量浓度范围内线性良好,吗啡、可待因在1.0~100.0 ng/mL范围内线性良好,r均大于0.999,方法检出限为0.3~2.5 ng/mL,定量限为1.0~7.5 ng/mL,5 种罂粟壳生物碱的平均回收率为85.8%~107.4%,相对标准偏差为0.5%~4.7%。该方法操作简单、净化效果好、检测效率高,适用于餐饮肉制食品中5 种罂粟壳生物碱的快速检测。  相似文献   

7.
目的 建立高效液相色谱-串联质谱法测定药酒中非法添加吗啡、可待因、蒂巴因、罂粟碱和那可丁5种罂粟壳生物碱的分析方法。方法 药酒在60 ℃水浴锅上挥去乙醇, 再加入含0.2%(V/V)甲酸的乙腈溶液提取, 最后用分散固相萃取(dispersive solid phase extraction, d-SPE)纯化管净化待测。以乙腈和10 mmol/L乙酸铵溶液(含0.1%甲酸)作为流动相进行梯度洗脱, 选用色谱柱为Xtimate TM C18柱, 在0.4 mL/min流速下, 质谱采用电喷雾电离源正离子扫描, 多反应监测模式检测。结果 吗啡和可待因线性范围为5.0~250.0 ng/mL, 蒂巴因、罂粟碱、那可丁的线性范围为1.0~50.0 ng/mL, 相关系数均在0.997以上。5种生物碱的方法检出限和定量限分别为0.02~0.80 μg/L 和 0.07~3.00 μg/L, 回收率范围为80.3%~101.5%, 相对标准偏差(relative standard deviation, RSD)在3.2%~8.1%之间(n=6)。结论 该方法简便、快速、准确可靠, 可用于药酒中罂粟壳生物碱含量的检测。  相似文献   

8.
目的建立检测火锅调料中非法添加罂粟壳(粉)的方法。方法样品经QuEChERS方法提取、净化后,采用超高效液相色谱串联三重四极杆质谱仪(UPLC.MS),在多反应监测(MRM)模式下,通过色谱、质谱条件优化及方法学考察,建立了高效、准确检测火锅调料中非法添加罂粟壳(粉)的方法。结果本方法的线性范围为:那可丁2.470~49.405ng/mL,r=0.9994;罂粟碱2.090~41.804ng/mL,r=0.9995;蒂巴因2.042~40.840ng/mL,r=1.000;可待因11.287~225.733ng/mL,r=0.9996;吗啡10.420~208.400ng/mL,r=0.9999。那可丁、罂粟碱、蒂巴因、可待因、吗啡的检测限分别为0.21,0.33,0.31,10.37,4.11μg/kg。回收率78.4%~100.6%。结论本方法快速、准确、灵敏度高,可用于检测火锅调料中的罂粟壳(粉)。  相似文献   

9.
目的:建立QuEChERS-超高效液相色谱-质谱联用法,测定酱卤肉中的吗啡、可待因、蒂巴因、罂粟碱、那可丁5种生物碱含量.方法 酱卤肉经QuEChERS法处理后,选择Waters Atlantis HILIC色谱柱,以10mmol/L甲酸铵溶液(含0.1%甲酸)和乙腈(含0.1%甲酸)作为流动相,以多反应监测(MRM)...  相似文献   

10.
建立了超高效液相色谱-串联质谱/质谱法高通量快速测定调料中吗啡、可待因、蒂巴因、罂粟碱、那可丁含量。样品通过乙腈一盐酸溶液提取,MCX固相萃取柱净化预处理后用超高效液相色谱-串联质谱/质谱仪进行检测。流动相为0.1%的乙酸-乙腈溶液+10mmol/L乙酸铵溶液,梯度洗脱,流速为0.2mL/min,柱温40℃。该方法对调料中罂粟碱、那可丁最低检出限分别为O.8、1.0μg/kg,吗啡、可待因和蒂巴因的最低检出限为50μg/kg,8min就可以全部检出。  相似文献   

11.
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.  相似文献   

12.
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.  相似文献   

13.
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.  相似文献   

14.
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.  相似文献   

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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.  相似文献   

18.
<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  相似文献   

19.
《印刷工业》2014,(11):95-95
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%.  相似文献   

20.
《印刷工业》2014,(8):103-103
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  相似文献   

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