固相分散萃取与气相色谱-负化学离子源质谱联用法测定食品中三唑醇的残留量

建立了食品中三唑醇残留量的固相分散萃取-气相色谱-负化学离子源质谱联用检测方法。样品中三唑醇残留物由正己烷饱和的乙腈(含1%冰醋酸)提取,加入无水硫酸镁与无水醋酸钠振荡促使提取液分层后进行固相分散萃取净化,用气相色谱-负化学离子源质谱法进行测定与确证,外标法定量。方法具有良好的选择性和抗干扰能力,其检出限和定量限分别为0.001 mg/kg和0.003 mg/kg;线性范围为0.050～0.750 mg/L,相关系数为0.9947;在0.005,0.010,0.020 mg/kg共3个添加水平下的平均回收率为70%～110%,相对标准偏差不大于12.0%。该方法适合于多种食品中三唑醇残留量的确证分析。     

液相色谱-串联质谱测定面条和米粉中的硫脲

建立了米面制品中硫脲的液相色谱-串联质谱(LC-MS/MS)测定方法.实验优化了样品提取方法、液相色谱条件和质谱参数.样品用80%乙醇超声波提取,离子交换色谱分离,色谱柱为NUCLEOSIL 100-5SA 阳离子交换柱,流动相为乙腈-(1%乙酸+0.2%乙酸铵)水溶液(30: 70),流速0.5mL/min.采用电喷雾质谱正离子模式电离,多反应选择离子检测,检测离子对为m/z 77/60和m/z 77/43,其中m/z 77/60为定量离子对.结果表明: 本方法简便快速、准确可靠,相对标准偏差＜4.0%;回收率为83%～90%;检出限为0.5 mg/kg;定量下限为 5 mg/kg.     

液相色谱-串联质谱法同时测定蔬菜中7种三唑醇类杀菌剂的残留量

采用高效液相色谱-串联质谱(HPLC-MS/MS)建立了同时测定蔬菜中环唑醇、三唑醇、粉唑醇、戊唑醇、己唑醇、烯唑醇和联苯三唑醇残留量的分析方法.样品经甲醇提取,分散固相萃取净化后,采用C8色谱柱(150 mm×2.1 mm,3 μm)分离,以甲醇-0.05%甲酸梯度洗脱,串联质谱测定,外标法定量.在优化实验条件下,7...     

高效液相色谱-串联质谱法测定蔬菜中氯虫苯甲酰胺和氟虫双酰胺残留

建立了蔬菜中氯虫苯甲酰胺和氟虫双酰胺残留量的高效液相色谱-串联质谱同时分析方法.蔬菜样品加入乙腈高速匀浆,提取液中加入无水MgSO4和NaCl,振荡离心后,取上清液稀释后直接进样,液相色谱-串联质谱电喷雾正离子扫描同时分析氯虫苯甲酰胺和氟虫双酰胺.以甘蓝、白菜、黄瓜、辣椒、番茄和茭白6种蔬菜为基质进行4个添加水平和5次重复性实验,结果表明, 添加浓度为0.01～5 mg/kg,蔬菜中氯虫苯甲酰胺和氟虫双酰胺添加回收率为85.4%～105%,相对标准偏差(RSD, n=5) 为2.5%～12%,氯虫苯甲酰胺和氟虫双酰胺的方法检出限(LOD)分别为0.0003 和0.002 mg/kg,定量限(LOQ)分别为0.001和0.006 mg/kg.本方法操作简单,灵敏度、回收率和重复性均良好.     

超高效液相色谱-串联质谱法测定果蔬中胺苯吡菌酮残留量

建立了一种超高效液相色谱-串联质谱(UPLC-MS/MS)法分析蔬菜和水果中胺苯吡菌酮残留量。用乙腈提取样品中残留的胺苯吡菌酮,提取液经十八烷基硅胶键合相(C18)和乙二胺-N-丙基硅烷(PSA)混合净化剂净化,使用UPLC-MS/MS电喷雾离子化、正离子扫描和多反应监测(MRM)模式检测,基质匹配标准溶液外标法定量。结果表明,胺苯吡菌酮在0.05～10μg/L范围线性关系良好,相关系数不低于0.9993。在0.1～2000μg/kg范围内,对黄瓜、菠菜、苹果、葡萄和洋葱样品进行添加回收率实验,平均回收率为81.2%～104.3%,相对标准偏差为2.2%～16%,方法的定量限为55 ng/kg,检出限为5.5 ng/kg。本研究建立的方法能对蔬果中胺苯吡菌酮残留量进行准确的定性和定量分析。     

超高效液相色谱-串联质谱法测定草鱼肉中阿苯达唑及其代谢物残留

建立了同时测定草鱼肉中阿苯达唑及其3种代谢物阿苯达唑亚砜、阿苯达唑砜、阿苯达唑-2-氨基砜的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。草鱼肉样品通过碱性乙酸乙酯提取,正己烷净化,超高效液相色谱分离,串联质谱检测,氘代同位素内标定量。本方法分析时间短,在4 min内即可完成4种被分析物的液质联用分析。本方法在0.1～10μg/kg范围内各物质线性良好,线性系数在0.9991～0.9996之间。阿苯达唑、阿苯达唑亚砜、阿苯达唑砜、阿苯达唑-2-氨基砜在0.5～5.0μg/kg添加水平下的平均回收率分别为98.4%～102.6%,97.1%～103.4%,98.8%～103.7%和101.1%～104.2%检出限分别为0.2,0.1,0.2和0.1μg/kg;日内精密度小于4.77%,日间精密度小于3.03%。本方法为阿苯达唑及其代谢物的检测及监控提供了一种快速、灵敏度高、重现性好的定量分析方法。     

化妆品中士的宁和马钱子碱的高效液相色谱检测及质谱确证

建立了高效液相色谱(HPLC)-二极管阵列检测器(DAD)测定化妆品中士的宁和马钱子碱的方法.膏霜、水剂、散粉、香波、唇膏等不同类型的化妆品样品经超声提取后,高效液相色谱-二极管阵列扫描检测,并在264 nm波长进行分析.用保留时间结合紫外光谱定性,外标法定量,并且采用液相色谱-质谱确证.士的宁的回收率为89.2%～103.5%,相对标准偏差在0.7%～6.0%之间,定量限为2.5 mg/kg,马钱子碱的回收率为86.3%～101.0%,相对标准偏差在0.9%～6.9%之间,定量限为2.5 mg/kg.     

液液萃取结合分散固相萃取-液相色谱串联质谱检测食品包装纸中的4-氨基偶氮苯

采用高效液相色谱-串联质谱法（LC-MS/MS）快速测定食品包装纸中偶氮染料释放的4-氨基偶氮苯.试样在0.5 mol/L氢氧化钠溶液的碱性环境下,用连二亚硫酸钠还原试样中的偶氮染料,用甲基叔丁基醚反萃取还原裂解产生的4-氨基偶氮苯,经氮吹、甲醇复溶后,用液相色谱-串联质谱进行测定,内标法定量.方法优化了色谱分离、质谱、液液萃取和分散固相萃取等条件.最优化条件下方法的检出限为0.13 mg/kg,定量限为0.42 mg/kg,加标回收率在90%~95%之间（添加水平分别为1、10、30 mg/kg）,相对标准偏差小于5%.     

固相萃取-气相色谱质谱联用法测定蔬菜中杜烯残留

建立固相萃取-气相色谱-质谱联用内标法测定蔬菜中杜烯残留量的检测方法.样品经乙腈提取,弗罗里硅土固相柱净化后,用气相色谱质谱联用仪进行检测.方法的检出限为0.005 mg/kg,经过不同实验室验证,样品中杜烯的平均基体添加回收率在81.0%～112.0%之间,室间精密度在1.03%～3.89%之间.     

高效液相色谱-电喷雾串联质谱法测定蜂蜜中5种头孢菌素

建立了用高效液相色谱-电喷雾串联质谱(LC-MS-MS)测定蜂蜜中5种头孢菌素残留量的方法.蜂蜜样品用磷酸盐缓冲溶液溶解,经Oasis HLB固相萃取柱净化.5种头孢菌素在C18柱上以乙腈-水为流动相梯度洗脱条件下完成分离,电喷雾电离串联质谱在正离子多反应监测模式下进行测定.添加浓度在2～100 μg/kg范围时,回收率为84.2%～103.6%; 相对标准偏差为3.89%～9.08%.本方法头孢唑啉的定量限为10 μg/kg, 头孢匹林、头孢氨苄、头孢洛宁、头孢喹肟的定量限为2.0 μg/kg.     

Multiresidue determination of 19 fungicides in processed fruits and vegetables by capillary gas chromatography after gel permeation chromatography.

A gas chromatographic (GC) method was developed for simultaneous determination of 19 fungicides (chlorothalonil, vinclozolin, dichlofuanid, triadimefon, penconazole, chlozolinate, captan, procymidone, triadimenol, folpet, hexaconazole, myclobutanil, cyproconazole, propiconazole, nuarimol, captafol, iprodione, fenarimol, and bitertanol) and the acaricide tetradifon in tomato puree, peach nectar, orange juice, and canned peas. Samples were extracted with acetone, partitioned with ethyl acetate-cyclohexane (50 + 50, v/v), and cleaned using gel permeation chromatography with ethyl acetate-cyclohexane (50 + 50, v/v) as eluant. The final extract was analyzed by GC with ion trap mass spectrometry (ITMS) using a DB5 capillary column. Recoveries from fortified samples ranged from 74.6 to 99.3%, except for triadimenol and bitertanol. Quantitation limits for most analytes were between 0.005 and 0.050 mg/kg. The purified extracts were analyzed further by GC with electron capture and nitrogen phosphorus detection, and the results were compared with those obtained by ITMS.     

GC/MS测定锅巴中丙烯酰胺含量

建立了一种测定市售锅巴中的丙烯酰胺含量的方法.该法样品前处理不必经过溴化衍生,样品脱脂后用水提取丙烯酰胺,提取液过活性炭柱,再用乙酸乙酯将活性炭柱中吸附的丙烯酰胺洗脱.洗脱液浓缩后经气相色谱-质谱(GC-MS)定量分析,检测限为0.06 mg/kg,适合测定市售锅巴中的丙烯酰胺的含量.还考察了丙烯酰胺在水的固液两相中的分配比.     

Evaluation of a method based on liquid chromatography/electrospray tandem mass spectrometry for analyzing eight triazolic and pyrimidine fungicides in extracts of processed fruits and vegetables

The feasibility of using liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) for determining 8 fungicides (triadimenol, penconazole, propiconazole, hexaconazole, cyproconazole, myclobutanil, fenarimol, and bitertanol) in extracts of tomato puree and lemon juice concentrate has been evaluated. A miniaturized extraction-partition procedure requiring small amounts of nonchlorinated solvents has been used. The extracts (5 microL) were analyzed by LC/ESI-MS/MS without any previous cleanup step. Chromatographic determination has been performed using a C18 column and isocratic elution. Seventeen MS/MS transitions of precursor ions were monitored simultaneously (2 or 3 for each pesticide). The excellent selectivity and good linearity of the LC/MS/MS method allowed quantitation and identification at low levels (limits of quantitation <0.010 mg/kg), even in difficult matrixes, with a run time of only 1.5 min.     

液相色谱-串联质谱法测定水稻中生长素及其氨基酸结合物

建立了同时测定水稻中吲哚-3-丁酸(IBA)、吲哚-3-乙酸(IAA)及其7种氨基酸结合物的液相色谱-串联质谱( HPLC - MS/MS)检测方法.样品在4℃下于80％甲醇中浸提12 h后,经混合阴离子交换反相固相萃取(MAX)净化,以5 mmol/L的甲酸铵溶液和甲醇为流动相,在C18柱上进行液相色谱分离,电喷雾正...     

蜂蜜中外源性γ-淀粉酶残留量的测定

采用液相色谱-同位素质谱联用法(LC-IRMS)建立了测定蜂蜜中外源性γ-淀粉酶残留量的方法。先采用凝胶色谱柱对蜂蜜样品进行预分离,将样品中所含的酶与糖分离开。根据γ-淀粉酶可将底物麦芽糖酶解为葡萄糖的原理,在55 ℃、pH 4.5的0.03 mol/L磷酸盐缓冲液中将γ-淀粉酶与麦芽糖反应48 h后,采用LC分离麦芽糖和葡萄糖,以IRMS测定酶解产物葡萄糖的含量来确定γ-淀粉酶的残留量。本方法的线性范围为5～200 U/kg,定量限为5 U/kg,回收率为89.6%～108.2%,相对标准偏差为3.3%～4.9%。采用本方法对市售蜂蜜和大米糖浆共38个样本进行了考察,γ-淀粉酶的检出率为76.3%。为了进一步验证本方法的检测能力,测定了掺入15%(质量分数)大米糖浆的蜂蜜样品,测得γ-淀粉酶的含量为10.2 U/kg。本方法能够有效地从酶学的角度鉴定蜂蜜中是否含有大米糖浆。     

固相萃取-高效液相色谱法同时测定大豆和大米中的磺酰脲类和二苯醚类除草剂残留

建立了大豆和大米中磺酰脲类和二苯醚类除草剂多残留同时检测的高效液相色谱分析方法。样品经乙腈提取,正己烷液-液分配,C18固相萃取小柱净化后,采用高效液相色谱方法分离,以乙腈-三乙胺盐酸溶液作流动相,梯度洗脱,紫外检测器检测。对样品前处理和色谱分析条件进行了优化,8种除草剂(甲磺隆、氯磺隆、苄嘧磺隆、吡嘧磺隆、三氟羧草醚、精恶唑禾草灵、乙氧氟草醚、乙羧氟草醚)在0.05~2.0 mg/L范围内线性关系良好。方法的定量限(S/N=10)为0.01~0.02 mg/kg,能达到国家有关上述除草剂残留限量的要求。大豆和大米样品的平均加标回收率分别为91.6%~116.1%和76.6%~110.8%,相对标准偏差(RSD)为1.0%~12.2%。所建立的方法在30 min内可完成一次检测,具有简便快速、灵敏可靠的特点,适用于大豆和大米中除草剂多残留的测定。     

Determination of fungicide residues in fruits by coupled-column liquid chromatography

Coupled-column liquid chromatography with fluorescence detection was applied to the determination of o-phenylphenol and bitertanol residues in orange and banana fruits. After extraction with a mixture of acetone, dichloromethane-petroleum ether, and ethyl acetate, an extract aliquot of 100 microL was injected directly without any additional clean-up into the chromatographic system using two reversed phase C18 coupled columns. The LC-LC approach allowed automated sample clean up of the vegetal extracts, leading to a simple and rapid analytical procedure, with limits of quantification between 0.01 and 0.05 mg kg(-1). Recovery experiments performed on orange and banana samples fortified at different concentrations (0.01 - 4 mg kg(-1)) gave average recoveries between 70 and 113% with relative standard deviations lower than 15%. The procedure developed was finally applied to orange and banana samples from different geographical locations and the results were confirmed by GC-MS.     

Analyses of pesticide residues in fruit-based baby food by liquid chromatography/electrospray ionization time-of-flight mass spectrometry

A liquid chromatography/electrospray ionization time-of-flight mass spectrometry (LC/ESI-TOFMS) method has been developed for the determination of 12 pesticides (namely, carbendazim, thiabendazole, imazalil, tridemorph, triadimefon, bitertanol, prochloraz, flutriafol, myclobutanil, iprodione, diphenylamine and procymidone) in fruit-based baby food (multi-fruit jars and juices intended for infant consumption). The developed method consists of a sample treatment step based on liquid-liquid extraction using acetonitrile, followed by a clean-up step based on dispersive solid-phase extraction (SPE) with a primary-secondary amine (PSA). Multi-fruit and apple juices were processed by a SPE procedure using Oasis HLB cartridges. Subsequent identification and quantitation was accomplished by LC/ESI-TOFMS analysis: the confirmation of the target pesticides was based on accurate mass measurements of selected ions (protonated molecules ([M+H]+) and fragment ions). Confirmation studies were accomplished at low concentration levels (10 microg kg-1) and accuracy errors lower than 2 ppm were obtained in most cases. Baby food extracts spiked at 10 microg kg-1 fortification level yielded average recoveries in the range 78-105% with relative standard deviations less than 10% for most of the analytes. Limits of detection (LODs) were between 0.1 and 4 microg kg-1 depending on the pesticide studied. Finally, the proposed method was applied to a total of 33 baby food samples from Spain and the United Kingdom. Although imazalil, thiabendazole and carbendazim were detected in a high number--over 60%- of baby food samples, none of the samples tested were found to be above the 0.01 mg kg-1 EU standard.     

分散固相萃取-高效液相色谱-质谱联用法测定水稻秸秆、糙米、稻壳和土壤中戊唑醇残留

建立了分散固相萃取-液相色谱-质谱法测定水稻秸秆、糙米、稻壳及土壤中戊唑醇残留量。方法以乙腈为萃取溶剂,N-丙基-乙二胺(PSA)为吸附剂,实现样品快速制备;在Zorbax Eclipse XDB-C18色谱柱上,以甲醇-5 mmol乙酸铵缓冲溶液(70/30,V/V)为流动相,采用电喷雾质谱检测器,选择离子监测模式,以m/z308为定量检测离子,戊唑醇保留时间在9.5 min左右,在0.005~2 mg/L范围内浓度与峰面积呈良好的线性关系,相关系数为0.9999。在4种样本中添加不同浓度戊唑醇其平均回收率在73.6%~105.8%,相对标准偏差(n=5)小于15%,检出限(S/N=5)为2.5×10-11g。该方法简单、快速、灵敏、准确。