Determination of carbofuran by GLC/NPD and HPLC in tomato fruits

Two analytical methods, using GLC/NPD and HPLC to analyse carbofuran residues in tomatoes, are described. Both methods have shown a high recovery rate, up to 90%, and their detection limits are below the maximum residue limit set by Codex Alimentarius Mundi for carbofuran in tomatoes. Therefore, both methods may be of use in routine analysis of this pesticide in those fruits.     

高效液相色谱法测定牛奶中速灭威、克百威、异丙威农药残留

建立了牛奶中速灭威、克百威（呋喃丹）、异丙威的高效液相色谱测定与确证方法。3种氨基甲酸酯类农药标准曲线线性关系良好;相关系数R2为0.990～0.996;检出限为6.13～7.87 μg/kg;回收率为70.4%～102.5%。该方法准确、灵敏、快速,可满足检测需要。     

Determination of ethychlozate and its degradation product in fruits by HPLC and LC/MS

A method was developed for the analysis of ethychlozate (CIE) and its decomposition compound, 5-chloro-3(1H)-indazolylacetic acid (CIA) in fruits by HPLC and LC/MS. The sample was homogenized with 1 mol/L HC1, and CIE and CIA were extracted with 5 mol/L HCl and acetone. They were extracted from the acetone extract with diethylether-n-hexane (2:1). CIE was hydrolyzed to CIA with methanol-4 mol/L KOH (1:1). The solution was made acidic, and CIA was extracted with diethylether-n-hexane (2:1). The extract was cleaned up on a silica gel column. CIA was determined by HPLC-UV and LC/MS (Scan or SIR). Four fruits were spiked with CIE or CIA at 0.5 microgram/g and analyzed by the proposed method with HPLC. The average recoveries were 77.2-83.2% for CIE and 71.2-89.2% for CIA. The concentrations determined by LC/MS were 10-25% higher than the values by HPLC. The limit of detection (LOD) of CIA standard solution by HPLC corresponds to 0.015 microgram/g of CIE in the sample. In the same way, the LOD of CIA by LC/MS (SIR) corresponds to 0.009 microgram/g of CIE in the sample.     

QuECHERS-高效液相色谱法测定西红柿、苹果、茶叶中的吡虫啉

本研究的目的是建立测定西红柿、苹果、茶叶中吡虫啉残留量的QuECHERS-高效液相色谱法(HPLC),通过加标测定出其回收率、精密度、检出限均在理想范围之内。具体测定方法为,样品经1%醋酸乙腈20mL、硫酸镁6g、醋酸钠1.5g,涡旋提取,离心,提取液经400mg PSA、400mg C18、1200mg MgSO4净化,吸取上清液上机测定。结果显示,吡虫啉在0.2~5.0mg/L范围内线性关系良好,R=0.9999,西红柿、苹果、茶叶基质回收率均在93%~100%范围内,西红柿、苹果检出限0.02mg/kg、定量限0.1mg/kg;茶叶检出限0.05mg/kg,定量限0.2mg/kg。     

UPLC-MS-MS法测定水产品中克百威及其代谢物

采用超高效液相色谱-串联质谱技术建立同时测定水产品中克百威及其代谢物(3-羟基克百威、3-酮基克百威和呋喃酚)含量的方法。样品经乙腈提取,正己烷脱脂,HLB固相萃取柱净化,色谱柱分离,电喷雾串联四极杆质谱进行检测,采用多反应监测分析,并对液质分离条件及参数和样品前处理条件进行优化。结果显示,克百威及其代谢物在0.08～100ng/mL范围内线性良好(0.998 3～0.999 7)。在0.25～2.5μg/kg时,平均加标回收率在87.9%～96.1%,RSD值在1.4%～9.5%。该方法测定克百威、3-羟基克百威、3-酮基克百威和呋喃酚的检出限均为0.25μg/kg。该方法快速、准确、灵敏,可用于水产品中克百威及其代谢物残留量的测定。     

Determination of acrylamide monomer in hydroponically grown tomato fruits by capillary gas chromatography—mass spectrometry

Tomato (Lycopersicon esculentum L) fruits from plants grown hydroponically on polyacrylamide gel were obtained in order to assess any possible uptake of acrylamide monomer from the nutrient solution to the fruit during cultivation. Analysis of acrylamide in the gel itself involved aqueous extraction, bromination and then capillary GC determination with nitrogen-specific detection. By standard addition a level of 0·18 ± 0·01 g kg^?1 residual monomer was found to be present in a sample of gel used by an experimental horticultural station. Tomato fruits were analysed by extraction of the aqueous phase, bromination, silica-gel cartridge clean-up and capillary GC–MS determination by selected ion monitoring. The recovery of the method was 26–62% but losses throughout were compensated for by use of 2,3-dibromo-2-dimethylpropionamide internal standard. No acrylamide monomer could be detected in tomato fruits from plants grown hydroponically on polyacrylamide gel at a limit of detection of 1 × 10^?6 g kg^?1, demonstrating that the monomer is not transferred from the growing medium into tomato fruits.     

高效液相色谱法测定玉米中西维因、呋喃丹含量的研究

介绍了西维因、呋喃丹的性质和最大残留量要求,研究并建立了高效液相色谱带紫外检测器分离测定呋喃丹、西维因的分析方法。经过多次试验测定,该方法具有前处理过程简单、分析速度快、结果准确、对仪器要求低等优点,较适合基层实验室使用。     

超高效液相色谱-串联质谱法测定果蔬中4种乙撑二硫代氨基甲酸酯农药残留

目的 建立超高效液相色谱-串联质谱法(UPLC-MS/MS)测定蔬菜、水果中4种乙撑二硫代氨基甲酸酯类农药残留量的方法。方法 试样采用L-半胱氨酸盐酸盐和碱性EDTA-Na₂溶液进行提取,碘甲烷衍生,QuEChERS原理净化浓缩,UPLC-MS/MS对乙撑二硫代氨基甲酸酯类农药衍生物进行测定,外标法定量。结果 水果的检出限为5μg/kg,蔬菜的检出限为10μg/kg,相关系数大于0.998,添加回收率的范围为82.3%～115.1%,相对标准偏差为2.3%～6.9%。结论 本文所建立的方法能够满足多种水果和蔬菜中乙撑二硫代氨基甲酸酯类农药快速准确检测。     

液相色谱-二极管阵列检测器测定大蒜中的蒜氨酸

建立液相色谱-二极管阵列检测器测定大蒜中蒜氨酸的分析方法.鲜蒜在脱氧水介质中,经微波灭酶后,用甲醇-水提取其中的蒜氨酸,以C18柱分离、二极管阵列检测器扫描检测.以保留时间和蒜氨酸的二阶导数光谱图定性,以215 nm波长下蒜氨酸峰面积定量.方法的线性范围为5.0～500.0μg/mL,加标回收率为93.2%～101.1%.     

凝胶渗透色谱-高效液相色谱法测定蔬菜中 呋喃丹的含量

目的建立凝胶渗透色谱-高效液相色谱法检测蔬菜中的呋喃丹农药残留量。方法样品经乙腈提取和环己烷-乙酸乙酯溶解后,经凝胶渗透色谱净化和反相高效液相C_(18)色谱柱分离后,采用荧光检测器进行测定,荧光检测激发波长为285 nm,发射波长为320 nm,采用高效液相色谱法以外标法定量。结果呋喃丹在0.2~5.0 ng/mL浓度范围内呈良好线性关系,相关系数r大于0.999,检测限为0.01 mg/kg。对空白蔬菜样品进行呋喃丹3个浓度水平0.5、1.0和2.0 mg/kg的加标,回收率结果为78.3%~97.6%,相对标准偏差为3.26%~11.69%。结论本研究所建立的方法简单、灵敏度高,可适用于蔬菜中的呋喃丹农药残留的分析检测。     

HPLC/MS测定白酒中的微量甜味剂

建立了测定白酒中微量甜蜜素、糖精钠、安赛蜜的HPLC/MS分析方法。样品用水适当稀释,直接进样测定。采用C18柱分高,在ESI负离子模式下检测。甜蜜素、糖精钠、安赛蜜测定的检出限分别为0.01、0.05和0.05mg/L,加标回收率分别为96.8%、96.0%和95.8%。     

HPLC-MS测定白酒中氨基甲酸酯类农药残留

建立了一种同时对白酒中10种氨基甲酸酯类农药残留的HPLC-MS测定方法。色谱条件:色谱柱Phenomenex-LunaCN100A(250mm×4.6mm×5μm),流动相乙腈-水(在40min内乙腈由20%变为80%),流速1.00mL/min,检测波长195nm,柱温25℃,进样量20μL。质谱条件:电喷雾离子源(ESI+源),扫描范围(m/z)为50～350,干燥气温度350℃,干燥气流速8.0mL/min,雾化气压力275.86kPa。样品制备:白酒样品用固相萃取处理后,氮吹浓缩,乙腈定容至2mL。结果表明,10种氨基甲酸酯类农药残留在0.05～3μg范围积线性关系良好,相关系数R2>0.99。平均回收率在72.6%和97.6%,RSD在2.6%～5.9%之间。结论:方法灵敏度高、操作简便、结果准确,可用于酒样中痕量农药残留的含量测定。     

番茄及其制品中番茄红素反相高效液相色谱法测定

建立了番茄及其制品中番茄红素高效液相色谱法测定方法.样品经丙酮加石油醚(2:1/V:V)(contain 0.1%BHT)提取,色谱柱采用(4.6×250 mm,i.d,5μm),流动相为甲醇-乙腈-二氯甲烷(体积比25:70:5),柱温为室温,检测波长为473 nm,番茄红素的保留时间为6 min.在3～24 mg/kg添加水平,回收率为87.8 %～99.9%,相对标准偏差为2.3%～5.8%.     

高效液相色谱-电喷雾质谱联用法检测大豆异黄酮和皂苷

应用高效液相色谱 电喷雾质谱联用法 ,直接对大豆胚芽的 70 %乙醇室温提取液进行检测 .根据各色谱峰的质谱特征 ,在室温提取液中鉴定出 9种异黄酮 ,7种A组皂苷 ,4种B组皂苷和2种E组皂苷 .结果证明对于复杂天然产物的定性定量分析 ,高效液相色谱 电喷雾质谱 (HPLC/ESI MS)联用分析法是一种方便快捷有效的方法 .     

邻-（2,3,4,5,6-五氟苄基）羟胺盐酸盐衍生-HPLC法测定果蔬中甲醛含量

通过邻-（2,3,4,5,6-五氟苄基）羟胺盐酸盐与甲醛衍生,建立了测定果蔬中甲醛含量的高效液相色谱法。样品在温度为70℃超声波条件下直接提取衍生30 min,经离心纯化后液相色谱检测,外标法定量。优化的色谱条件为:Eelipse XDB-C₁₈柱（4.6 mm×250 mm,5μm）;流动相为乙腈和水（70∶30,v/v）,流速1.0 m L/min,柱温40℃,检测波长210 nm。结果表明,该方法的检出限可达到0.114 mg/kg,在0.57⁵7 mg/kg范围内呈良好的线性关系,平均回收率为82.3%⁹4.1%,相对标准偏差为4.0%⁷.1%（n=6）。该方法样品前处理简便,稳定性好,检测限低,适合果蔬中甲醛的快速定量检测。      

QuEChERS-HPLC测定柚类果实中柠檬苦素类化合物

建立了柠檬苦素类化合物的QuEChERS-HPLC检测方法,同时测定了不同品种柚类果实中柠檬苦素、诺米林、黄柏酮3种柠檬苦素类化合物含量。样品经乙腈均质超声提取,离心后取上清液,用QuEChERS净化管净化,通过CAPCELL PAK C₁₈ MG色谱柱(250 mm×4.6 mm, 5μm)梯度洗脱分离,检测波长为210 nm,二极管阵列检测器。结果表明,方法在0.10～200μg/mL线性良好,相关系数大于0.999,平均回收率为99.0%～100.3%,相对标准偏差为1.0%～2.1%。柚类果实不同品种以及不同果实组织部位中3种柠檬苦素类化合物含量差异显著。该研究可为柠檬苦素类化合物在食品和医药等领域的利用研究提供参考。     

超高效液相色谱法测定水果中咪鲜胺残留量

建立了水果中咪鲜胺残留量的超高效液相色谱（UPLC）检测方法。样品经乙腈提取,PCX固相萃取柱净化后,以甲醇-水（70∶30, V/V）为流动相,在流速1.0 mL/min条件下等度洗脱,检测波长为 225 nm,用UPLC法快速测定水果中咪鲜胺残留量。在0～5.0 μg/mL范围内,咪鲜胺的峰面积与其质量浓度呈线性相关,相关系数R≥0.999 7,在香蕉、苹果和柑橘中分别添加0.2 mg/kg、0.4 mg/kg、1.0 mg/kg 3个质量浓度的咪鲜胺标准品,回收率为93.00%～101.10%,精密度实验结果相对标准偏差（RSD）为0.219%,方法检出限为0.032 mg/kg。该方法能满足水果中咪鲜胺残留量检测要求。     

液相色谱-质谱联用测定食品中的微量甜蜜素

建立测定食品中微量甜蜜素的液相色谱-质谱测定方法.样品中的甜蜜素用水提取,经C18柱分离后,用ESI负离子模式检测.方法的线性范围为1.0～100.0 ng/mL,检出限为0.01μg/g,加标回收率为92.0%～102.0%.     

Simultaneous determination of pesticide residues in fruits and vegetables by GC/MS (SCAN mode) and HPLC

A method was developed for simultaneous determination of pesticide residues in fruits and vegetables. Residues were extracted from samples with acetonitrile, followed by a salting-out step and a partitioning step with n-hexane at the same time. Co-extractives were removed with ENVI-Carb/LC-NH2 mini-column cleanup. Analysis was performed by GC/MS (SCAN mode) and HPLC. Of the 139 pesticides spiked at 0.1 or 0.5 microgram/g into 6 fruits and vegetables (spinach, tomato, apple, radish, cabbage and carrot), recoveries of 117 pesticides were between 70 and 120%. This method is appropriate for determining these pesticides and for screening several other pesticides for which the recoveries were < or = 70% or > or = 120% (imazalil, etc.). The limits of detection for most pesticides in this method were equal to or lower than those of the bulletin method in Japan.     

液相色谱串联质谱法测定再造烟叶中的甲基异噻唑啉酮及其氯代物

建立了液相色谱串联质谱测定再造烟叶中的甲基异噻唑啉酮及其氯代物的方法。样品用甲醇做萃取剂,经涡旋振荡,C8 液相色谱柱分离,串联质谱仪MRM 模式检测。结果发现,在0.05~l0mg/L 范围内线性良好,定量限分别为2.5 μg/L、2.8 μg/L,回收率分别为95.2%、92.3%,相对标准偏差<5%。该方法操作简单、效率高、适合推广运用。