加速溶剂萃取-高效液相色谱法测定土壤中的亚当氏剂

加速溶剂萃取仪(ASE)提取土壤中亚当氏剂残留的最佳条件为:甲醇作提取剂,萃取温度90℃,压力为10689.7kPa(1550psi),样品经提取、浓缩后,以高效液相色谱测定含量.方法简便、快速,对土壤中亚当氏剂的回收率为81.2%～102.5%,相对偏差为5.4%,检出限为0.091mg/L.     

加速溶剂萃取-高效液相色谱串联质谱法测定土壤中邻苯二甲酸酯

建立了高效液相色谱串联质谱技术(Liquid chromatography tandem mass spectrometry,LC-MS/MS)同时测定土壤中邻苯二甲酸酯(Phthalic acid esters,PAEs)的分析方法。确定了土壤样品加速溶剂萃取最优条件是以正己烷为萃取溶剂,在160℃下,静态萃取4次,每次12 min,萃取液经旋转蒸发浓缩,以乙腈-0.1%甲酸溶液为流动相梯度洗脱分离后,用LC-MS/MS结合大气压化学源(Atmospheric pressure chemical ionization,APCI)进行定性及定量分析。土壤中11种PAEs的浓度与其峰面积呈良好的线性关系,检出限为0.03~13.0μg/kg,样品的加标平均回收率为72.8%~101.8%,相对标准偏差(RSD)为1.7%~6.7%。方法简便快速,且灵敏度高,适用于土壤中11种邻苯二甲酸酯的同时测定。     

离子液体-加速溶剂萃取-高效液相色谱法测定蜜饯中的有机酸类防腐剂

以离子液体氯化1-辛基-3-甲基咪唑盐([Omim]Cl)的水溶液为萃取剂,采用加速溶剂萃取结合高效液相色谱法测定了蜜饯中苯甲酸、山梨酸、肉桂酸等有机酸类防腐剂,优化了加速溶剂萃取实验参数,最佳萃取条件为:离子液体浓度为0.1mol/L,萃取时间为5min,萃取温度为80℃。在最佳条件下,有机酸类防腐剂的检出限为0.4～27.7μg/L。将本方法用于蜜饯样品的检测,回收率为78.2%～113.9%。实验结果表明:离子液体-加速溶剂萃取法快速、高效。     

加速溶剂萃取-气相色谱法测定土壤中的联苯菊酯

建立了加速溶剂萃取-色谱法测定土壤中的联苯菊酯残留量的方法.土壤样品与无水硫酸钠以1∶2(质量比)混合后,再加适量中性氧化铝,用丙酮-石油醚(体积比为1∶1)在加速溶剂萃取仪上以10.3 MPa、80℃提取5 min,Florisil小柱净化,然后采用ECD气相色谱测定,在0.56、1.12 μg/kg两个添加水平下,联苯菊酯的加标回收率为72.7%～87.2%,检出限为0.1 μg/kg.测定结果的相对标准偏差为9.3%(n=8).该法能有效地消除复杂基质带来的干扰,可以作为日常样品中联苯菊酯残留量的检测和确证方法.     

加速溶剂萃取-高效液相色谱法测定塑料制品中多溴二苯醚

提出了塑料制品中多溴二苯醚的高效液相色谱法。样品经粉碎后用乙醇-丙酮(1+1)萃取溶剂经加速溶剂萃取仪在150℃静态萃取10min,提取液旋转蒸发后用正己烷溶解过硅胶固相萃取柱净化,流出液蒸发至近干用异辛烷-甲苯(4+1)混合溶剂定容后,注入高效液相色谱仪分离测定。方法的检出限(3S/N)在0.1～0.2mg.L-1之间,加标回收率在87%～104%之间。     

全自动加速溶剂萃取-高效液相色谱-串联质谱法测定土壤中6种抗生素的残留量

随机选取代表性土壤样品约1 kg,四分法将土壤样品缩分,取约200 g风干、粉碎、过筛。取上述土壤样品10.0 g置于萃取池中,加入硅藻土15.0 g混合均匀后进行加速溶剂萃取(ASE),采用凝胶净化系统净化提取液。取净化液10 mL,于50℃氮吹至近干,残渣用1 mL甲醇溶解,过0.22μm滤膜,采用高效液相色谱-串联质谱法(HPLC-MS/MS)测定其中林可霉素、克林霉素、洛美沙星、培氟沙星、恩诺沙星和环丙沙星等6种抗生素的含量,质谱分析采用多反应监测模式。结果表明,6种抗生素的质量浓度在0.001～1.0 mg·L^-1内与对应的峰面积呈线性关系,检出限(3S/N)为0.004～0.019μg·kg^-1。方法用于分析单标准溶液和加标样品溶液,所得测定值的相对标准偏差(n=6)均小于4.0%。按标准加入法进行回收试验,回收率为83.8%～105%。方法用于实际样品分析,6种抗生素的检出量为15.7～221.6μg·kg^-1。     

加速溶剂萃取-高效液相色谱法测定皮革和纺织品中含氯苯酚的含量

建立了测定皮革和纺织品中含氯苯酚的高效液相色谱/二极管阵列检测器(HPLC/DAD)分析方法.采用加速溶剂萃取法萃取不同类型的皮革和纺织品样品,以正己烷为提取剂,在10.34 MPa和120 ℃下静态循环提取3次,提取液经氮吹仪浓缩近干,以正己烷溶解并定容;采用C18柱,以乙腈/0.5%乙酸溶液为流动相,DAD波长为214 nm进行高效液相色谱分离与分析.结果表明: 四氯苯酚和五氯苯酚质量浓度在0.1～20 mg/L范围内具有良好的线性关系(r＞0.9999);平均回收率在 96.0%～101.5% 之间;相对标准偏差为 0.50%～5.5% (n=7);方法的检出限为0.02 mg/kg,符合欧盟指令0.05 mg/kg的限量规定.本方法高效、简便、自动化程度高,准确可靠,是一种可同时快速测定皮革和纺织品中含氯苯酚的新方法.     

全自动加速溶剂萃取-超高效液相色谱-串联质谱法测定土壤中7种杀线虫剂的残留量

通过优化提取、净化条件,提出了题示方法测定土壤样品中棉隆、噻唑膦、灭线磷、丰索磷、杀线威、丁硫环磷、除线磷等7种杀线虫剂的含量。随机采集土壤样品,风干,粉碎后过筛,分取10.0 g,加入硅藻土15.0 g,用体积比2:1的甲醇和三氯甲烷混合溶液进行加热加压全自动萃取;萃取液过活化好的HLB固相萃取柱,用10 mL体积比1∶1的甲醇和乙腈混合溶液洗脱。洗脱液于45℃氮吹至近干,残留物用1 mL乙酸乙酯溶解,过0.22μm滤膜,滤液采用超高效液相色谱-串联质谱法测定。结果显示：7种杀线虫剂的质量浓度在0.005～2.0 mg·L^-1内与峰面积呈线性关系,检出限(3S/N)为4～25μg·kg^-1;按照标准加入法进行回收试验,回收率为87.2%～101%,测定值的相对标准偏差(n=6)为1.5%～3.8%;方法用于实际样品分析,检出了棉隆、噻唑膦、灭线磷、丰索磷、除线磷,检出量为14.81～124.03μg·kg^-1。     

加速溶剂萃取-凝胶色谱净化高效液相色谱法测定动物源性食品中的胆固醇

采用加速溶剂萃取-凝胶色谱净化建立了动物源性食品中胆固醇检测的高效液相色谱方法。结果表明,胆固醇浓度在1.0~40.0mg/L范围内线性关系良好,加标回收率为89.1%~99.8%,相对标准偏差为3.1%~7.8%。该方法准确、灵敏度高,适用于富含脂类的动物源性食品中胆固醇的检测。     

加速溶剂萃取/超高压液相色谱-质谱联用对土壤中甲胺磷的测定研究

建立了加速溶剂萃取/超高压液相色谱-质谱联用测定土壤中甲胺磷的方法。确定最佳萃取条件为:萃取溶剂为乙腈,萃取温度80℃,静态萃取时间10 min,循环2次。萃取液经旋转蒸发仪浓缩后,进超高压液相色谱-质谱分析,外标法定量,质谱定性。结果表明,甲胺磷的线性范围为3.15~1 050μg/L,相关系数为0.999 1。低、中、高3个加标水平下甲胺磷的平均回收率为72%~82%,相对标准偏差为5.8%~8.6%,检出限为0.05μg/kg。该方法具有良好的分离效果、较宽的线性范围和较高的灵敏度,可用于实际样品检测。     

快速溶剂萃取-毛细管电泳法测定土壤和底泥中磺胺类药物残留

建立了一种快速溶剂萃取(ASE)-毛细管电泳检测土壤和底泥中磺胺类药物残留的新方法。通过优化ASE的萃取条件,选取甲醇为萃取剂,在70℃、10.3 MPa的条件下提取土壤和底泥样品中的磺胺类药物。毛细管电泳检测磺胺嘧啶,磺胺甲基嘧啶和磺胺间二甲氧基嘧啶的标准曲线具有良好的线性(r>0.999)。方法的定量限(LOQ,S/N=10)为0.056～0.070 mg/kg。日内相对标准偏差在0.4%～2.5%之间,日间相对标准偏差在1.2%～4.6%之间。3个加标水平0.100、0.625、2.50 mg/kg的平均回收率在82%～103%之间,RSD≦4.3%。方法已用于土壤和底泥样品前处理和磺胺类药物残留检测。     

Determination of imazethapyr and imazapyr residues in soil by coupled-column liquid chromatography

Summary A column-switching method using two separation columns combined with UV detection at 260 or 236 nm has been used to determine the imidazolinone herbicides imazethapyr and imazapyr in soils. The residues were extracted from the soil with 0.1 M aqueous sodium carbonate solution and, after adjusting the pH to 2.0, the solution was partitioned with dichloromethane. Limits of determination for imazethapyr and imazapyr were 3 μg/kg. Recoveries were from 55 to 75% for both imidazolinone herbicides in the range 3–100 μg/kg in soil.     

Rapid screening of dioxin-contaminated soil by accelerated solvent extraction/purification followed by immunochemical detection

Since soils at industrial sites might be heavily contaminated with polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs), there is a need for large-scale soil pollution surveys and, thus, for cost-efficient, high-throughput dioxin analyses. However, trace analysis of dioxins in complex matrices requires exhaustive extraction, extensive cleanup, and very sensitive detection methods. Traditionally, this has involved the use of Soxhlet extraction and multistep column cleanup, followed by gas chromatography—high-resolution mass spectrometry (GC/HRMS), but bioanalytical techniques may allow much more rapid, cost-effective screening. The study presented here explores the possibility of replacing the conventional method with a novel approach based on simultaneous accelerated solvent extraction (ASE) and purification, followed by an enzyme-linked immunosorbent assay (ELISA). Both the traditional and the novel cleanup and detection approaches were applied to contaminated soil samples, and the results were compared. ELISA and GC/HRMS results for Soxhlet-extracted samples were linearly correlated, although the ELISA method slightly underestimated the dioxin levels. To avoid an unacceptable rate of false-negative results, the use of a safety factor is recommended. It was also noted that the relative abundance of the PCDDs/PCDFs, evaluated by principal component analysis, had an impact on the ELISA performance. To minimize this effect, the results may be corrected for differences between the ELISA cross-reactivities and the corresponding toxic equivalency factor values. Finally, the GC/HRMS and ELISA results obtained following the two sample preparation methods agreed well; and the ELISA and GC/HRMS results for ASE extracts were strongly correlated (correlation coefficient, 0.90). Hence, the ASE procedure combined with ELISA analysis appears to be an efficient approach for high-throughput screening of PCDD-/PCDF-contaminated soil samples.      

Rapid selective accelerated solvent extraction and simultaneous determination of herbicide atrazine and its metabolites in fruit by ultra high performance liquid chromatography

A selective accelerated solvent extraction procedure achieved one step extraction and cleanup for analysis of herbicide atrazine and its metabolites in fruit. Using a BEH C18 analytical column and the gradient mode with 2 mM ammonium acetate aqueous solution/acetonitrile as a mobile phase achieved effective chromatographic separation of the five analytes within 4 min. The calibration curves were linear over two orders of magnitude of concentration with correlation coefficients (r) of 0.9996?0.9999. The method limit of quantification was 1, 2, 1.5, 3, and 2 μg/kg for atrazine, desethylatrazine, desisopropylatrazine, desethyldesisopropylatrazine, and hydroxyatrazine, respectively, in the case of atrazine it is at least two orders of magnitude lower than the maximum residue limit (0.25 mg/kg). The intra‐day and inter‐day precisions of the five analytes were in the range of 2.1–3.5 and 3.1–4.8 %, respectively. The recoveries of the five analytes at three spiked levels varied from 85.9 to 107% with a relative standard deviation of 1.8–4.9% for pear and apple samples. The ultra high performance liquid chromatography with diode array detection method was proved to be fast, inexpensive, selective, sensitive, and accurate for the quantification of the analytes in pear and apple samples.     

Influence of processing procedure on the quality of Radix Scrophulariae: A quantitative evaluation of the main compounds obtained by accelerated solvent extraction and high‐performance liquid chromatography

An improved high‐performance liquid chromatography with diode array detection combined with accelerated solvent extraction method was used to simultaneously determine six compounds in crude and processed Radix Scrophulariae samples. Accelerated solvent extraction parameters such as extraction solvent, temperature, number of cycles, and analysis procedure were systematically optimized. The results indicated that compared with crude Radix Scrophulariae samples, the processed samples had lower contents of harpagide and harpagoside but higher contents of catalpol, acteoside, angoroside C, and cinnamic acid. The established method was sufficiently rapid and reliable for the global quality evaluation of crude and processed herbal medicines.     

快速溶剂萃取-高效液相色谱法测定含脂羊毛中残留的除虫脲和杀铃脲

建立了快速溶剂萃取-高效液相色谱(ASE-HPLC)测定含脂羊毛中除虫脲、杀铃脲残留量的方法。以正己烷饱和的乙腈为萃取剂,在80 ℃、10.34 MPa条件下用快速溶剂萃取仪提取样品中的目标物,提取液经冷冻除脂、浓缩及Waters Plus Silica柱净化后,采用Waters Atlants dC18色谱柱分离,以乙腈和水为流动相进行梯度洗脱,二极管阵列检测器于254 nm处检测。结果表明,在0.1～10.0 mg/L范围内,除虫脲、杀铃脲的峰面积与其质量浓度的线性关系良好,相关系数均大于0.9999,定量检出限(S/N≥10)分别为0.05,0.04 mg/kg。该方法具有操作简便、快速、灵敏度高等特点,完全能满足含脂羊毛中除虫脲、杀铃脲残留初筛检测的要求。     

加速溶剂萃取-快速液相色谱法测定纺织品中烷基苯酚和烷基苯酚聚氧乙烯醚

建立了纺织品中烷基苯酚和烷基苯酚聚氧乙烯醚的加速溶剂萃取-快速液相色谱测定方法。加速溶剂萃取法基本实现了样品前处理的自动化,简化了操作流程;快速液相色谱分析方法(利用核壳型快速分析色谱柱)大大缩短了样品分析时间(色谱分析时间小于5 min)。该方法在提高工作效率的同时节省了有机溶剂,且易于在普通实验室普及的常规液相色谱仪上实现,具有较强的实用性。     

加速溶剂萃取-气相色谱-负化学源质谱法测定茶叶中有机氯和拟除虫菊酯类农药残留量

建立了茶叶中13种有机氯和10种拟除虫菊酯农药残留量的气相色谱-负化学离子源.质谱(GC-NCl-MS)分析方法.茶叶样品用V(丙酮):V(CH2Cl2)=1:1混合液作提取剂经加速溶剂萃取,提取液经凝胶色谱净化除去大部分的色素、脂类和蜡质,再经活性炭-氨基(Carb-NH2)复合小柱和Florisil小柱净化后,用GC-NCl-MS的选择离子监测方式(SIM)进行定性和定量分析.添加50μg/kg 浓度水平时,农药回收率在45.6%～112.4%之间,相对标准偏差在0.57%～10.1%之间;方法的检出限(3倍信噪比)在0.05～10.0μg/kg之间.方法适用于出口茶叶农残检测实际工作.     

Interfacing ASE and HPLC for the Determination of PAH in Soil

A method was developed to couple an accelerated solvent extraction system (ASE) with high performance liquid chromatography (HPLC) for the analysis of PAH in soil samples. The resolution of HPLC is well maintained while the advantages of ASE, fast extraction, less solvent consumption and ease of operation, are well expressed. The precision and accuracy of this method are verified by a series of analyses of reference material, and the precision of retention from multiple injection indicates minimum loss of chromatographic resolution by the interface of this technique. Detection limits for the studied PAH range from 0.07 ng/Kg to 0.21 ng/Kg with a fluorescence detector.