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1.
建立了不同食品接触材料中5种乙醇胺类化合物迁移量的液相色谱-串联质谱(LC-MS/MS)测定方法。以5种不同食品模拟物(水、4%乙酸、10%乙醇、50%乙醇、95%乙醇)浸泡样品,4%乙酸浸泡液经氮气吹干后用水复溶,其他浸泡液直接过滤后进样。采用氨基柱BEH Amide(50 mm×2.1 mm,1.7μm)分离,以乙腈-5 mmol/L乙酸铵溶液为流动相,梯度洗脱分离,在电喷雾源的正离子多反应监测(MRM)模式下检测,外标法定量。在优化条件下,5种乙醇胺类化合物在1.0~750.0μg/L范围内线性关系良好,相关系数均大于0.997,检出限(LOD,S/N=3)和定量下限(LOQ,S/N=10)分别为0.3~5.0μg/kg和1.0~15.0μg/kg。在1.0~750.0μg/kg加标水平下的回收率为90.2%~118%,相对标准偏差(RSD)为0.5%~8.8%。该方法高效灵敏、准确可靠,可满足相关检测的需求。  相似文献   

2.
以乙酸乙酯为萃取溶剂对染整助剂中残留的乙二醇醚及其醋酸酯进行超声萃取后,经Waters Sep-Pak Vac Silica(1 g/6 mL)固相萃取柱净化,选用DB-Wax色谱柱(60 m×0.25 mm×0.25μm)分离,采用气相色谱-串联质谱(GC-MS/MS)方法进行多反应监测(MRM)分析,外标法定量,建立了同时测定染整助剂中15种乙二醇醚和4种乙二醇醚醋酸酯的分析方法。结果显示,19种待测物峰面积(A)与其质量浓度(ρ)在一定范围内呈线性相关,相关系数均不低于0.999 2。分别以3倍信噪比(S/N=3)和S/N=10计算方法检出限(LOD)和定量下限(LOQ),得MOPA和DEGME的LOD均为30μg/kg,DEGDEE的LOD为20μg/kg,EGEE和EGME的LOD均为10μg/kg,其余14种目标分析物的LOD为1~5μg/kg;MOPA和DEGME的LOQ均为100μg/kg,EGEE、EGME和DEGDEE的LOQ分别为20、30、50μg/kg,其余14种目标分析物的LOQ为1~15μg/kg。在低、中、高3个加标浓度水平下的平均加标回收率为82.4%~94.6%,相对标准偏差为2.7%~9.2%。该方法操作简单、灵敏度高、定量下限低,完全满足染整助剂中乙二醇醚及其醋酸酯残留量检测工作的需要。  相似文献   

3.
采用高效液相色谱-四极杆/离子阱质谱(HPLC-QTRAP-MS)建立了面粉及面制品中氨基脲的确证及测定方法。样品采用盐酸(HCl)提取,在超声辅助下与衍生剂邻硝基苯甲醛反应。衍生产物在中性条件下经PLS固相萃取柱净化、乙酸乙酯洗脱,经Shim-Pack XR-ODSⅢC18柱(2.0 mm×50 mm,1.6μm)分离,0.1%(体积比)甲酸-水溶液和甲醇溶液为流动相梯度洗脱;采用多反应监测(MRM)-信息依赖性采集(IDA)-增强子离子扫描(EPI)模式检测,EPI谱库确认,内标法定量。结果表明:氨基脲在0.5~40μg/L范围内线性关系良好(r=0.996);检出限(LOD,S/N=3)为0.10μg/kg,定量下限(LOQ,S/N=10)为0.25μg/kg;4个加标水平(0.25,0.5,2.0,10.0μg/kg)下的回收率为89.1%~112.8%;相对标准偏差(RSD)为1.4%~8.6%。该方法分析速度快,灵敏度高,回收率好,可用于面粉及面制品中氨基脲的快速检测。  相似文献   

4.
建立了水产品中巴龙霉素、壮观霉素、妥布霉素、庆大霉素、卡那霉素、潮霉素B、安普霉素、链霉素、双氢链霉素、丁胺卡那霉素和新霉素共11种氨基糖苷类药物(AGs)残留的超高效液相色谱-串联质谱(UPLCMS/MS)检测方法。样品经磷酸盐缓冲液提取,分子印迹聚合物(MIP)固相萃取柱净化,Obelisc R色谱柱分离,采用超高效液相色谱-串联质谱仪进行测定。方法检出限(LOD,S/N≥3)为1.0~10.0μg/kg,定量限(LOQ,S/N≥10)为2.0~20.0μg/kg。11种AGs在1.0~1000μg/kg范围内线性关系良好(R20.994),在水产品中加标回收率为78.4%~109.6%,相对标准偏差(RSD,n=6)为2.3%~14.9%。本方法灵敏度高,且可实现11种AGs同时检测。  相似文献   

5.
气相色谱法测定坚果中8种拟除虫菊酯农药残留   总被引:1,自引:0,他引:1  
建立了东盟进口坚果夏威夷果、开心果、杏仁中8种拟除虫菊酯农药残留的检测方法。样品采用乙腈作萃取溶剂超声波提取,经中性氧化铝串联弗罗里硅土小柱净化,组分经不同极性的两根毛细管柱进行分离,采用气相色谱法以ECD检测器检测坚果中8种拟除虫菊酯农药。该方法在0.01~1.0μg/m L浓度范围内具有良好的线性关系,相关系数为0.999 2~0.999 9;在农药添加浓度为10,20,50μg/kg时,回收率为71%~115%,相对标准偏差为4.5%~9.8%,检出限(LOD,S/N=3)为0.014~0.28μg/kg,定量下限(LOQ,S/N=10)为0.047~0.94μg/kg。该方法分离效果好,准确可靠,回收率高,方便快速,可用于坚果中农药残留的日常检测。  相似文献   

6.
建立了鹅组织(肌肉、肝脏、肾脏以及皮肤和脂肪)中哌嗪残留的气相色谱-串联质谱检测法。鹅组织经加速溶剂萃取(ASE350),乙腈提取,过Strata-X-C固相萃取小柱净化后的样品在乙酸酐和三乙胺条件下衍生。衍生产物经气相色谱-串联质谱仪(GC-MS/MS)检测,色谱柱为TG-5MS Amine(30 m×0.25 mm i.d.,0.25μm),载气为氦气,进样口和检测器温度均为280℃。采用EI模式,SCAN和SIM扫描定性,Auto SRM结合外标法定量。哌嗪添加量在5.1~2.5×10~3μg/kg范围内,线性关系良好,相关系数为0.9995。在定量限(LOQ:5.1,5.2,5.2,5.2)~2.0×10~3μg/kg的加标水平上,鹅组织中哌嗪的平均回收率为85.2%~95.5%,相对标准偏差(RSD)为1.6%~4.7%,日内RSD为1.2%~5.3%,日间RSD为2.0%~7.7%。检测限(LOD)和定量限(LOQ)分别在1.4~1.6μg/kg(S/N≥3)和5.1~5.2μg/kg(S/N≥10)之间。方法适用于鹅组织中哌嗪残留的检测。  相似文献   

7.
郑阳  许秀丽  纪顺利  袁飞  黄志强  杨丙成  张峰 《色谱》2016,34(5):512-519
利用固相萃取结合气相色谱-串联质谱(SPE-GC-MS/MS)检测技术建立了烟草制品中23种酯类香料的定量分析方法。样品以乙酸乙酯为提取溶剂,经NH2固相萃取柱(依次用甲醇和水活化)净化,用4 mL乙酸乙酯洗脱,在多反应监测(MRM)模式下进行检测。结果表明,23种香料在20.0~500.0 μ g/L范围内线性关系良好(r2 > 0.996),检出限(LOD, S/N=3)及定量限(LOQ, S/N=10)分别为1.9~13.6 μ g/kg及6.3~45.3 μ g/kg,在1、1.5、2倍定量限的加标水平下,平均回收率为62.1%~91.4%,相对标准偏差(RSD)均小于7%。该方法准确可靠、灵敏度好,适用于烟草制品中23种常用酯类香料的快速筛查与定性、定量分析。该方法为烟草中酯类物质的检测开拓了平台。  相似文献   

8.
建立了水产品中亮绿、亚甲基蓝及其代谢物残留量同时测定的液相色谱-串联质谱(LC-MS/MS)方法。样品经乙酸铵缓冲溶液和乙腈提取,二氯甲烷液液萃取,PRS固相萃取柱净化,氮吹浓缩,定容后测定。以2 mmol/L乙酸铵(含0. 1%甲酸)、乙腈和甲醇为流动相,CAPCELL PAK C_(18)色谱柱进行分离,在选择反应监测(SRM)模式下测定,外标法定量。在最佳实验条件下,5种化合物在1. 0~100. 0μg/L范围内线性关系良好(r~2 0. 999),检出限(LOD,S/N≥3)均为1. 0μg/kg,定量下限(LOQ,S/N≥10)均为2. 0μg/kg;在水产品中加标水平为1. 0、5. 0、10. 0μg/kg时,回收率为70. 3%~92. 1%,相对标准偏差(RSD,n=6)为2. 3%~13%。该方法灵敏度高,能有效检测水产品中亮绿、亚甲基蓝及其代谢物的残留量。  相似文献   

9.
高效液相色谱-串联质谱法测定蜂蜜中20种全氟烷基化合物   总被引:1,自引:0,他引:1  
李帅  陈辉  金铃和  彭涛  范春林  王明林 《色谱》2017,35(5):495-501
建立了高效液相色谱-串联质谱(HPLC-MS/MS)同时测定蜂蜜中20种全氟烷基化合物(PFASs)含量的分析方法。采用改进的QuEChERS方法对样品进行前处理,用含1.5%(v/v)甲酸的乙腈溶液振荡提取,C_(18)和N-丙基乙二胺(PSA)吸附剂净化,Atlantis T3 C_(18)色谱柱(150 mm×2.1 mm,3μm)分离,以含5 mmol/L乙酸铵的甲醇溶液和5 mmol/L乙酸铵溶液为流动相进行梯度洗脱。在电喷雾离子(ESI)源负离子模式下以多反应监测(MRM)扫描,采用同位素内标法进行定量分析。结果表明,20种PFASs在16 min内即可完成分离,在0.2~10μg/L范围内线性关系良好,相关系数(r)均大于0.99;检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.04~0.10μg/kg和0.10~0.20μg/kg。在0.1、0.5、1.0和2.0μg/kg加标水平下,20种PFASs的加标回收率为72.6%~113.0%,RSD为0.4%~15.9%(n=6)。该法快速、高效、准确,适用于蜂蜜样品中20种PFASs的同时检测。  相似文献   

10.
《色谱》2015,(8)
建立了一种分子印迹固相萃取-超高效液相色谱-串联质谱同时测定猪肉中5种β2-受体激动剂残留的方法。样品经过均质处理后置于乙酸铵/乙酸缓冲液中,加入内标物和β-葡萄糖醛酸酶/芳基硫酸酯酶,于55℃酶解2 h,调节溶液p H后通过分子印迹固相萃取柱净化,然后采用BEH C18色谱柱分离,以甲醇-0.1%(v/v)甲酸水溶液为流动相,采用梯度洗脱,在电喷雾正离子多反应监测模式下用内标法定量。检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.005~0.009μg/kg和0.015~0.025μg/kg。在0~10μg/kg范围内线性关系良好,相关系数≥0.993 3。添加水平为0.25、1、5μg/kg时,回收率为80.4%~92.9%,相对标准偏差为1.2%~6.3%。该方法具有灵敏度高、重复性好、回收率高等优点,适合同时进行多种β2-受体激动剂残留的测定。  相似文献   

11.
Preparation, Crystal Structures, Vibrational Spectra, and Normal Coordinate Analysis of four Linkage Isomeric Trichlorotrirhodanoosmates(IV) By treatment of fac-[OsCl3I3]2? with (SCN)2 in dichloromethane the linkage isomers fac-[OsCl3(NCS)3]2? ( 1 ), mer-[OsCl3(NCS)2c(SCN)]2? ( 2 ), mer-[OsCl3(NCS)(SCN)2t]2? ( 3 ), and mer-[OsCl3(NCS)(SCN)2c]2? ( 4 ) are formed which have been separated by ion exchange chromatography on diethylaminoethyl cellulose. X-Ray structure determinations have been performed on single crystals of fac-(Ph4As)2[OsCl3(NCS)3] (triclinic, space group P1 , a = 12.142(5), b = 13.233(5), c = 19.300(5) Å, α = 98.642(5)º, β = 100.509(5)º, γ = 112.514(5)º, Z = 2), mer-(Ph4As)2[OsCl3(NCS)2c (SCN)] · acetone (triclinic, space group P1 , a = 11.707(5), b = 13.238(5), c = 19.048(5) Å, α = 75.960(5)º, β = 88.981(5)º, γ = 69.999(5)º, Z = 2), mer-(Ph4As)2[OsCl3(NCS)(SCN)2 t] (triclinic, space group P1, a = 10.6861(12), b = 11.6587(5), c = 12.5232(5) Å, α = 112.069(8)º, β = 95.052(8)º, γ = 92.559(7)º, Z = 1) and mer-(Ph4As)2[OsCl3(NCS)(SCN)2 c] · 2acetone (triclinic, space group P1 , a = 11.444(5), b = 14.661(5), c = 15.830(5) Å, α = 75.790(5)º, β = 80.273(5)º, γ = 75.205(5)º, Z = 2). The complex anions are completely ordered. The via N or S coordinated thiocyanate groups are located nearly direct above one of the cis-positioned Cl ligands with Os? N? C angles of 169.1º, 171.5º, 175.7º ( 1 ), 175.6º, 178.6º ( 2 ), 172º ( 3 ), and 173.1º ( 4 ) and Os? S? C angles of 106.2º ( 2 ), 106.1º, 106.6º ( 3 ), 105.1º, and 108.2º ( 4 ). Using the molecular parameters of the X-Ray determinations the low temperature (10 K) IR and Raman spectra of the (n-Bu4N) salts of all four linkage isomers have been assigned by normal coordinate analyses based on a modified valence force field. The valence force constants are fd(OsN) = 1.71 ( 1 ), 1.46 and 1.62 ( 2 ), 1.69 ( 3 ), and 1.61 ( 4 ), fd(OsS) = 1.27 ( 2 ), 1.36 ( 3 ), 1.32, and 1.49 mdyn/Å ( 4 ). Taking into account increments of the trans influence a good agreement between observed and calculated frequencies is achieved.  相似文献   

12.
Preparation, Crystal Structures, Vibrational Spectra, and Normal Coordinate Analysis of Four Linkage Isomeric Tetrachlorodirhodanoosmates(IV) By treatment of cis- or trans-[OsCl4I2]2? with (SCN)2 in dichloromethane the linkage isomers cis-[OsCl4(NCS)2]2? ( 1 ), trans-[OsCl4(NCS)(SCN)]2? ( 2 ), cis-[OsCl4(NCS)(SCN)]2? ( 3 ) and trans-[OsCl4(SCN)2]2? ( 4 ) are formed which have been separated by ion exchange chromatography on diethylaminoethyl cellulose. The X-Ray structure determinations on single crystals of cis-(Ph4As)2[OsCl4(NCS)2] (triclinic, space group P1 , a = 10.019(5), b = 11.702(5), c = 21.922(5) Å, α = 83.602(5)°, β = 85.718(5)°, γ = 73.300(5)°, Z = 2), trans-(Ph4As)2[OsCl4 · (NCS)(SCN)] (monoclinic, space group P21/c, a = 18.025(5), b = 11.445(5), c = 23.437(5) Å, β = 94.208(5)°, Z = 4), cis-(Ph4As)2[OsCl4(NCS)(SCN)] (triclinic, space group P1 , a = 10.579(5), b = 11.682(5), c = 22.557(5) Å, α = 81.073(5)°, β = 85.807(5)°, γ = 87.677(5)°, Z = 2) and trans-(Ph4As)2 · [OsCl4(SCN)2] (triclinic, space group P1 , a = 10.615(5), b = 11.691(5), c = 11.907(5) Å, α = 111.314(5)°, β = 96.718(5)°, γ = 91.446(5)°, Z = 1) reveal the complete ordering of the complex anions. The via N or S coordinated thiocyanate groups are located nearly direct above one of the cis-positioned Cl ligands with Os? N? C angles of 171.2° and 174.3° ( 1 ), 162.3° ( 2 ), 172° ( 3 ) and Os? S? C angles of 108.3° ( 2 ), 105.7° ( 3 ) and 105.5° ( 4 ). Using the molecular parameters of the X-Ray determinations the low temperature (10 K) IR and Raman spectra of the (n-Bu4N) salts of all four linkage isomers are assigned by normal coordinate analyses based on a modified valence force field. The valence force constants are fd(OsN) = 1.59 ( 1 ), 1.67 ( 2 ), 1.60 ( 3 ) and fd(OsS) = 1.27 ( 2 ), 1.31 ( 3 ) and 1.32 mdyn Å?1 ( 4 ). Taking into account increments of the trans influence a good agreement between observed and calculated frequencies is achieved.  相似文献   

13.
Preparation and Crystal Structure of (n-Bu4N)3[Ir(NCS)(SCN)5] The evaporated ethanolic extrakt of the reaction product of K3[IrCl6] and HNO3, refluxed with an aqueous KSCN solution yields a mixture of the linkage isomers [Ir(NCS)n(SCN)6?-n]3?, n = 0? 2, and small amounts of linkage isomeric chloropentarhodanoiridates(III), from which [Ir(NCS)(SCN)5]3? has been isolated by ion exchange chromatography on DEAE-cellulose. The X-Ray structure determination on a single crystal of (n-Bu4N)3[Ir(NCS)(SCN)5] (monoclinic, space group P 21/a, a = 17.513(5), b = 32.607(5), c = 23.661(5) Å, β = 94.757(5)°, Z = 8) confirms the existance of a heteroleptic hexakis(thiocyanato(N)-thiocyanato(S))iridate(III) with an Ir? N distance of 2.03 Å and Ir? S bond lengths between 2.29 and 2.38 Å. The SCN groups with angles between 166 and 175° are nearly linear with Ir? S? C angles from 99.9 to 109.4°. The Ir? N? C angles of the two crystallographic independent anions are 166 and 174°.  相似文献   

14.
Thermogravimetry (TG) was employed to study the thermal degradation kinetics of poly(etherketone/sulfone)ethylimide (PEK-IE and PES-IE). The corresponding decomposition activation energies and reaction orders were obtained and the comparison was made with their parent polymerspoly(ether-ketone/sulfone) with Cardo group (PEK-C and PES-C). The results show that the degradation activation energies of PEK-IE and PES-IE were lower than that of PEK-C and PES-C; and two stages of the degradation process were found for all the four polymers. For PEK-IE and PES-IE, the activation energies in the first decomposition stage are much lower than that in the second stage and the two stages can be taken as slow induction and fast degradation, whereas for PEK-C and PES-C the activation energies in the first decomposition stage are larger than that in the second stage, and the two stages can both be taken as two fast degradation stages. The decomposition mechanism of the two stages was also speculated.This revised version was published online in November 2005 with corrections to the Cover Date.  相似文献   

15.
Abstract

The reaction, in water, of Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) ions with sodium ampicillinate at room temperature has allowed isolation of dimers with the following general formula [M(amp)Cl]2 × nH2O (n = 1.5?3.2). The complexes were characterized by elemental analyses, conductivity measurements, magnetic susceptibilities and spectroscopic methods (IR, Raman, EPR and UV-Visible). A dinuclear structure based on octahedrally coordinated metal ions is proposed.  相似文献   

16.
高原  张茂根  王昉  王炳祥  沈健 《应用化学》2005,22(10):1096-1099
PMDA-BPDA-HAB聚苯并噁唑的合成及耐热性;均苯四甲酸二酐;联苯四羧酸二酐;二羟基联苯胺;聚酰亚胺;聚苯并噁唑;耐热性  相似文献   

17.
Summary: The thermal degradation behavior of poly(ε-caprolactone) (PCL) and poly(L-lactic acid) (PLA) have been studied in different environment. It was found that these polymers undergo completely different degradation processes in nitrogen and oxygen atmosphere. In oxygen environment PCL and PLA mainly decompose to CO2, CO, water and short-chain acids. In nitrogen atmosphere PCL releases 5-hexenioc acid, CO2, CO and ε-caprolactone, whereas PLA decomposes to acetaldehyde, CO2, CO and lactide. The polymer blends of poly(3-hydroxybutyrate) (PHB) with PCL and PLA decompose similar to the individual homopolymers with crotonic acid as the initial decomposition product of PHB.  相似文献   

18.
In this paper, we carry out the calculation on the system (X@C60)(X=Li, Na, K, Kb, Cs; F, Cl, Br, I), where the position of X changes along 5 typical symmetry directions. For the calculation of quantum chemistry we use EHMO/ASED method, for the calculation of molecular mechanics we use Buckingham potential (exp-6-1) function, and for the calculation of thermo-chemical cycle we use individually isolating the processes such as the structure variation, charge transfer and charge distribution, and their interactions etc. The calculation results show that (1) In the region of radius r≈0.2 nm of the Ceo cage, the potential field is nearly spherical; (2) Except for Li and Na, the systems are the most stable with minimum energies at the center of C60 cage. For Li and Na, the systems are the most stable with minimum energies at r≈0.16 nm and r≈0.13 nm, respectively. In view of the interactive region of chemical bonds, the interactions between X and the C60 cage do not belong to the classical chemical bonds; (  相似文献   

19.
Cu以其优异的导电性、导热性和易加工性广泛用于工农业生产中.自然Cu的腐蚀和防腐成为人们很关注的问题.人们已经注意到,Cl-对Cu的腐蚀有影响,并进行过一些研究.但目前使用光电化学方法研究这一问题的文章尚不多见,特别是利用测量开路光电压及其瞬态波形这一现场的、无损的、灵敏的监测方法研究户对Cu电极腐蚀全过程的文章尚未见到.本文正是利用如上方法及XPS,AES方法,研究了Cl-对Cu电极腐蚀的全过程,取得了一些有意义的结果.1实验方法Cu电极用99.99%(质量分数)的Cu制成,面积约为39mm2;电极底部由Cu导线焊接引出,…  相似文献   

20.
Fundamental understanding of microphase separation in ABC miktoarm copolymers is vital to access a plethora of nonconventional morphologies. Miktoarm stars based on poly(cis 1,4-isoprene) (I), poly(styrene) (S), and poly(2-vinylpyridine) (V) are model systems, which allow systematic studies of the effects of composition, chemical microstructure, and temperature on the thermodynamics of microphase separation. Eleven ISV-x (I:S:V = 1:1:x, v:v:v) miktoarm copolymers were synthesized by anionic polymerization affording well-defined copolymers with a variable V arm. Equilibrium bulk morphologies of all samples, as evidenced by small-angle X-ray scattering, transmission electron microscopy (TEM), and self-consistent field theory, showed a systematic transition from lamellae (x ≈ 0–0.2) to [8.8.4] tiling (x ≈ 0.6–0.9) to cylinders in undulating lamellae (x ≈ 2–4) and, finally, to hexagonally packed core–shell cylinders (x ≈ 5–8). Chemical microstructure of the I arm [poly(cis 1,4-isoprene)] versus poly(3,4-isoprene) is shown to play important role in affecting morphological behavior. To reconcile differences between ISV-x star morphologies reported in the literature and those reported herein, even for the same composition, effects of the microstructure of I arm on the Flory–Huggins parameter between I and V arms were taken into account in a qualitative manner. © 2018 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2018 , 56, 1491–1504  相似文献   

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