正化学源-气相色谱-质谱法测定食用植物油中有机锡化合物残留

建立了正化学源-气相色谱-质谱技术测定食用植物油中有机锡化合物残留的方法。食用油样品经环己烷-乙酸乙酯（1：1，v/v）溶解后，经凝胶渗透色谱（GPC）净化，目标馏分用四乙基硼酸钠进行衍生。采用基质校正曲线外标法定量，在20~2000 μg/L范围内，7种有机锡化合物均呈现良好的线性关系，相关系数大于0.99，定量限为0.3~1.2 μg/kg。对芝麻油样品进行加标回收试验，在0.05、0.10、0.20 mg/kg 3个添加水平下，7种有机锡化合物的平均回收率为66.2%~103.2%，相对标准偏差均小于11.5%。该方法精密度好，灵敏度高，可用于食用植物油中有机锡化合物残留量的测定。     

气相色谱-质谱法分析蜂蜜中多种有机氯农药残留

建立了气相色谱-电子轰击离子化-质谱法（GC-EI-MS）同时分析蜂蜜试样中12种有机氯农药残留的分析方法.蜂蜜试样用V（正己烷）：V（乙酸乙酯）=5：1混合提取剂超声提取和Florisil硅藻土层析柱净化后,以PCB 103为内标物,采用GC-EI-MS的选择离子监测方式（SIM）分析,同时探讨了一些有机氯农药EI-MS特征离子的结构与断裂机理.当空白试样的加标浓度为10、50、200μg/kg时,加标回收率为80%～112%,相对标准偏差为0.4%～9.8%,方法检出限为0.2～4.0μg/kg,其中8种农药的MDL＜1.0μg/kg,线性范围为10～500μg/kg,相关系数皆大于0.996,此方法已用于蜂蜜试样中多种痕量有机氯农药残留的分析.     

高效液相色谱-串联质谱法测定化妆品中壬基苯酚

提出了高效液相色谱-串联质谱法测定化妆品中壬基苯酚含量的方法。化妆品试液用甲醇-二氯甲烷（8+2）混合溶液超声提取30 min[唇膏类试样用无水乙醇-二氯甲烷（8+2）混合溶液],离心分离取上清液过Oasis HLB固相萃取柱净化。从SPE净化柱所得淋出液,以WatersXBridge C₁₈色谱柱（2.1 mm×150 mm,3.5μm）为固定相分离,以不同体积比的甲醇和氨水（0.1+99.9）溶液为流动相梯度洗脱,串联质谱进行测定。采用电喷雾负离子模式多反应监测,内标法定量。壬基苯酚的线性范围为10～500μg·L^-1,测定下限（10S/N）为0.2 mg·kg。方法用于分析4种类型化妆品样品,回收率在83.1%～103.0%之间,相对标准偏差（n=6）在2.75%～9.24%之间。     

凝胶色谱-高效液相色谱法测定茶叶中蒽醌

建立了用凝胶渗透色谱-高效液相色谱测定茶叶中蒽醌的方法。以乙酸乙酯、乙酸乙酯-正己烷(1∶1,V/V)液液萃取,凝胶渗透色谱净化,收集时间为11~17 min,以甲醇+0.5%H3PO4溶液(65+35,V/V)为流动相,ZORBAX SB-C18分离,外标法定量。蒽醌质量浓度在10~200μg/L范围内线性关系良好,相关系数r为0.9993,检出限为6μg/kg,定量限为10μg/kg。茶叶样品在10,50,180μg/kg 3个加标浓度下,蒽醌的回收率为73.2%~97.5%,相对标准偏差为4.0~7.9%。     

高效液相色谱-串联质谱法检测中药材中有机磷农药残留量

研究了中药材中有机磷农药残留量的高效液相色谱-串联质谱同步检测方法.采用CAPCELL PAK MC C18反相柱,以乙腈为提取溶液,以Carb/PSA柱为净化柱,液相色谱-串联质谱仪测定.方法线性范围为10～500 μg/L,11种有机磷农药在此范围内线性良好,相关系数为0.9961～0.9999.在10～100 μg/kg浓度范围内,加标回收率在70%～110%之间,相对标准偏差为1.4%～11%,最低检出限为2～20μg/kg,符合残留检测分析要求.     

固相萃取净化-气相色谱/串联质谱法测定茶叶中54种农药残留量

建立了固相萃取净化-气相色谱/串联质谱(SPE-GC-MS/MS)分析茶叶中54种农药残留的方法。样品用乙睛提取,提取液经石墨化炭黑/氨基固相萃取柱净化后,采用气相色谱-串联质谱方法在分时段选择反应监测模式下进行测定,外标法定量。当54种农药加标水平为10、50、100μg/kg时,回收率为60%～150%,方法的相对标准偏差小于16%;定量限(LOQ)均小于10μg/kg;在20～320μg/L范围内线性关系良好。方法已用于同时检测茶叶中农药多残留。     

多功能针式过滤器净化超高效液相色谱法测定大米和花生中玉米赤霉烯酮

建立了一种基于多功能针式过滤器净化的超高效液相色谱测定大米和花生中玉米赤霉烯酮的方法。样品经乙腈提取,采用多功能针式过滤器通过式净化,以超高效液相色谱法测定其中的玉米赤霉烯酮,色谱柱为ACQUITY UPLC BEH C18柱（100 mm×2.1 mm,1.7μm）,以甲醇-乙腈-水（体积比为8∶46∶46）为流动相等度洗脱,流量为0.3 mL/min,用荧光检测器检测,色谱峰面积外标法定量。玉米赤霉烯酮的质量浓度在2.5～500 ng/mL范围内与色谱峰面积线性关系良好,相关系数不小于0.999 5。大米和花生样品的方法检出限分别为15.0、30.0μg/kg,定量限分别为50.0、100.0μg/kg。样品加标回收率为77.11%～93.65%,测定结果的相对标准偏差为0.49%～4.95%(n=6)。该方法简便快速,适用于大米和花生中玉米赤霉烯酮的日常检测。     

蜂蜜中泰妙菌素残留量的高效液相色谱-串联质谱法测定

建立了固相萃取-高效液相色谱-串联质谱(HPLC-MS/MS)测定蜂蜜中泰妙菌素残留量的分析方法。样品用甲醇-偏磷酸水溶液提取,OasisMCX SPE小柱净化,经C18色谱柱分离,以电喷雾离子源在正离子多反应监测(MRM)模式下进行测定,外标法定量。泰妙菌素的方法检出限为0.04μg/kg,定量下限为0.1μg/kg,在0.5～50μg/L范围内线性关系良好,相关系数r为0.999 8。在0.1～5.0μg/kg加标水平内泰妙菌素的回收率为80%～94%,RSD为4.5%～8.1%。该方法实用、准确、灵敏,适用于蜂蜜中泰妙菌素残留量的测定。     

液相色谱串联质谱测定畜禽肉中黄霉素A的残留量

建立了高效液相色谱串联质谱法测定畜禽肉中黄霉素A残留量的方法,样品中残留的黄霉素A经提取,HLB柱净化后,以Agilent Ecillps C18色谱柱为分析柱,乙腈-10 mmol/L的乙酸铵为梯度洗脱液,经串联四极杆质谱多反应监测模式检测,黄霉素A得到了很好的分离。线性范围为10～1000μg/kg。黄霉素A的定量限为10μg/kg。添加浓度在10～50μg/kg时,回收率在70%～100%之间,变异系数在4.6%～8.8%之间。方法适合出口畜禽肉及组织中黄霉素A残留量的测定。     

凝胶渗透色谱-超高效液相色谱-串联质谱法测定水产品中多种同化激素残留

结合凝胶渗透色谱净化技术,建立了超高效液相色谱-串联质谱法测定水产品中6种同化激素的残留。样品经叔丁基甲醚提取,以乙酸乙酯-环己烷(1+1)溶液为流动相进行凝胶渗透色谱净化,用C18固体吸附剂净化,以C18色谱柱分离,采用电喷雾正离子源、多反应监测模式检测,外标法定量。6种激素的线性范围均为0.5~50μg·L-1,测定下限(10S/N)在0.20~1.50μg·kg-1之间。对空白样品进行加标回收试验,回收率在81.7%~90.8%之间,日间精密度(n=5)在5.8%~7.9%之间。     

土壤中64种痕量半挥发性有机污染物的分析方法研究

利用超声提取技术将土壤中的半挥发性有机污染物(SVOC)提取出来, 经旋转蒸发浓缩至一定体积后, 用ODSC18柱净化, 再用氮吹浓缩后, 取1.0 μL注入气相色谱中, 用DB-5 ms柱分离, 用气相色谱质谱仪(GC-MS)进行定性定量分析. 本方法研究土壤中64种半挥发性有机污染物, 其中包括苯系物、苯酚类、苯胺类、硝基芳香烃类、氯代芳烃类、多环芳烃类和酞酸酯类等物质的提取、净化方法以及回收率、精密度和检测限的测定. 该方法回收率为52.5%～105%.     

固相萃取-高效液相色谱法测定浓缩苹果汁中的多菌灵残留量

报道了固相萃取-高效液相色谱法测定浓缩苹果汁中多菌灵残留量的方法.样品经适量水稀释后,C18固相萃取柱提取净化,用V(甲醇)∶V(二氯甲烷)=1∶1淋洗,HPLC法测定.在添加水平为0.10,0.50,2.0 mg/kg时,多菌灵的回收率在92.6%～108.3%之间;RSD＜3% (n=6),检出限为0.02 mg/kg,该方法的测定结果满足农药残留量的检测要求.     

烤鳗中6种农药残留量的液相色谱-质谱/质谱法同时测定

建立了烤鳗中苯胺灵、嘧菌酯、氨苯乙酯、氟酮唑草、丙蝇驱、唑螨酯6种农药残留的同时检测方法.烤鳗样品采用乙腈、中性氧化铝超声基体分散吸附、涡旋混合提取,Florisil固相萃取小柱净化、浓缩,以乙腈-乙酸铵缓冲液为流动相进行色谱分离,串联质谱检测.结果表明,6种化合物在0.5 ～1 000 μg/L范围内线性关系良好,方法的检出限为0.03 ～2.3 μg/kg,定量下限为0.09 ～7.7 μg/kg,平均加标回收率为75% ～104%,相对标准偏差(RSD)为1.6% ～15%,满足当前进出口残留控制要求.     

竹笋中40种农药残留的固相萃取/气相色谱-质谱法同时测定

建立了竹笋中40种农药(包括有机磷类、有机氯类、氨基甲酸酯类、拟除虫菊酯类、三唑类和杂环类)残留的同时检测方法.样品以乙腈为提取溶剂,高速匀浆提取,经PSA固相萃取小柱净化,利用GC-MS/SIM进行测定.结果表明,40种农药在一定质量浓度范围内线性良好,相关系数为0.994 6 ～0.999 8.在0.050 ～2....     

超高效液相色谱-串联质谱法同时测定食品中碱性橙、碱性嫩黄O和碱性桃红T

本文建立了同时测定食品中碱性橙、碱性嫩黄O和碱性桃红的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法.样品经碱化甲醇提取、二氯甲烷萃取、浓缩、酸化甲醇溶解和甲醇饱和正己烷溶液萃取净化后进行测定.本方法检出限分别为碱性橙0.6 μg/kg、碱性嫩黄O 0.3 μg/kg、碱性桃红T 0.7 μg/kg.六种食品样品的回收率为72.1%～91.1%,相对标准偏差(RSD)为2.4%～9.1%(n=6),三种染料在0.01～0.5 μg/mL范围内呈良好的线性关系,线性回归系数r均大于0.9950.     

超高效液相色谱-电喷雾离子源-串联三重四极杆质谱分析人血中羟基多溴联苯醚

建立了超高效液相色谱-电喷雾离子源串联三重四极杆质谱(UPLC-ESI-MS-MS)在负离子模式下测定人血中5种羟基多溴联苯醚(HO-PBDEs)的方法.血清样品中加入替代内标13C<,12四溴双酚-A(13C<,12TBBP-A),经萃取、净化、浓缩等预处理过程,多重反应监测(MRM),扫描通道为:m/z 555→4...     

A new cleanup method of dioxins in sediment using large volume injection gas chromatography online coupled with liquid chromatography

A new cleanup method was developed and validated for the determination of polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans (PCDD/Fs) in sediment. The sample extract was first treated with sulfuric acid and then cleaned up by a large volume injection gas chromatography online coupled with liquid chromatography (LVI-GC-LC) system. PCDD/Fs in the extract were separated by a GC column (DB-5), selected cut, cool trapped and transferred to a LC column (alumina). The fraction of PCDD/Fs eluted from the alumina column was collected and concentrated for the instrumental analysis. Under the optimized conditions, LVI-GC-LC method achieved the recoveries of 57–102% for 2,3,7,8-substituted PCDD/Fs, which met the requirements of US Environmental Protection Agency (EPA) Method 1613 and were better than those obtained using the conventional multistep column cleanup method. Meanwhile, compared with the conventional method, the limit of detection (LOD) values of 2,3,7,8-substituted PCDD/Fs cleaned up by LVI-GC-LC method were decreased due to the high-efficiency removal of interferents. These results suggested that the LVI-GC-LC cleanup method was a promising alternative to the multistep cleanup procedure for the determination of dioxins in environmental samples.     

固相萃取-HPLC法同时测定浓缩柑橘汁中噻菌灵、多菌灵的残留量

建立了一种可同时测定浓缩柑橘汁中噻菌灵和多菌灵残留量的反相HPLC分析法。浓缩柑橘汁样品用水适当稀释后,经过调节pH值、离心、过滤,用混合相固相萃取小柱(m ixed-mode SPE)进行提取、净化,用配有二级管阵列检测器(DAD)的液相色谱仪检测,外标法定量。使用噻菌灵和多菌灵对照品进行添加回收试验,噻菌灵、多菌灵的回收率分别为80.8%~87.1%、82.9%~87.7%,二者的测定下限均为0.020 mg/kg,测定结果的相对标准偏差均不大于7.38%(n=10)。     

Determination of residues of 446 pesticides in fruits and vegetables by three-cartridge solid-phase extraction-gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry

A method was developed for determination of residues of 446 pesticides in fruits and vegetables through the use of cleanup by a 3-cartridge solid-phase extraction-gas chromatography/ mass spectrometry (GC/MS) and liquid chromatography/tandem mass spectrometry (LC/MS/MS). Fruit and vegetable samples (20 g) were extracted with 40 mL acetonitrile, salted out, and centrifuged. Half of the supernatant was passed into an Envi-18 cartridge, eluted with acetonitrile, and cleaned up with Envi-Carb and aminopropyl Sep-Pak cartridges in series after concentration of the eluates. Pesticides were eluted with acetonitrile-toluene (3 + 1, v/v), and eluates were concentrated to 0.5 mL and then added into internal standards after solvent exchange with 2 mL hexane and used for determination of 383 pesticides by GC/MS. The other half of the supernatant was concentrated to 1 mL and cleaned up with Envi-Carb and aminopropyl Sep-Pak cartridges in series. Pesticides were eluted with acetonitrile-toluene (3 + 1, v/v), and the eluates were concentrated to 0.5 mL, dried with nitrogen gas, diluted to 1.0 mL with acetonitrile-water (3 + 2, v/v), and used for determination of 63 pesticides by LC/MS/MS. The limit of detection for the method was 0.2-600 ng/g depending on the individual pesticide. In the method, fortification recovery tests at high, medium, and low levels were conducted on 6 varieties of fruits and vegetables, i.e., apples, oranges, grapes, cabbage, tomatoes, and celery, with average recoveries falling within the range of 55.0-133.8% for 446 pesticides, among which average recoveries between 60.0-120.0% accounted for 99% of the results. The relative standard deviation was between 2.1-39.1%, of which a relative standard deviation of 2.1-25.0% made up 96% of the results. Experiments proved that the method was applicable for determination of residues of 446 pesticides in fruit and vegetables.     

Reversed-phase high-performance liquid chromatographic determination of linear alkylbenzenesulphonates in river water at ppb levels by precolumn concentration.

A high-performance liquid chromatography method for the determination of linear alkylbenzenesulphonates (LASs) in river waters has been developed. The ppb levels of LASs can be determined by reversed-phase high-performance liquid chromatography with ultraviolet detection after on-line anion-exchange concentration and successive injection. LASs were quantitatively concentrated on the anion-exchange precolumn and easily cleaned up from river water matrix, because of its specific affinity, for the anion-exchange resin. A weak non-polar reversed-phase column was useful for the determination of LASs. The relationships between concentration and summation of peak areas were linear from 10 to 200 ppb for total LAS concentrated from 5 ml of standard solutions. Overall recovery for total LAS was found to be 99%. Total LAS in the Tama River waters was determined to be around 100 ppb by the proposed method.