Solid phase extraction of methomyl and thiodicarb from environmental water with an activated carbon cartridge and their determination by HPLC

A solid phase extraction procedure of methomyl and thiodicarb from environmental water was presented. This method utilizes a 40—60 mesh activated carbon cartridge and high performance liquid chromatography (HPLC). The 40—60 mesh activated carbon works faster and yield higher adsorption efficiency. Detection limits of methomyl and thiodicarb in environmental water are 0 1 μg/L and 0 2 μg/L, respectively. Average recoveries of fortified methomyl and thiodicarb in water are in the range of 90 7%—98 8% and 88 9%—103 6%, respectively. The relative standard deviations are lower than 7%. This method is simple, rapid, accurate and precise.

Determination of Eleutheroside B and E in Acanthopanax Preparations by High-P erformance Liquid Chromatography with Solid-Phase Extraction

Aim An HPLC method for analyzing eleutheroside B (ELU B) and eleutheroside E(ELU E) , two of the main active substances of Acanthopanax preparations were studied. Methods Thesamples were analyzed on a kromasil ODS column with water-acetonitrile as a gradient mobile phase.The flow rate was 0.8 mL·min^(-1) and detecting wavelengths were 206 nm for ELU B, 220 nm for ELUE, solid phase extraction (SPE) and internal standard-salicin were selected. Results The recoveriesof Acanthopanax tablets and injection were 90.4% - 96.8% and 96.4% - 99.8% for ELU B, 87.7% -93.3%and 95.7% - 98.5% for ELU E, respectively. The linear ranges were 4.45 - 22.25 μg· mL^(-1) (r =0.999 8) and 5.11 - 25.55 μg·mL^(-1) ( r = 0.999 7) respectively. Conclusion This method can savethe time for cleaning the chromatographic system and improve sensitivity for Acanthopanaxpreparations , thus providing a way to evaluate the quality of Acanthopanax preparations.

Determination of Triclocarban, Triclosan and Methyl-Triclosan in Environmental Water by Silicon Dioxide/Polystyrene Composite Microspheres Solid-Phase Extraction Combined with HPLC-ESI-MS

This paper developed a sensitive and efficient analytical method for triclocarban (TCC), triclosan (TCS) and Methyl-triclosan (MTCS) determination in environmental water, which involves enrichment by using silicon dioxide/polystyrene composite microspheres solid-phase extraction and detection with HPLC-ESI-MS. The influence of several operational parameters, including the eluant and its volume, the flow rate and acidity of water sample were investigated and optimized. Under the optimum conditions, the limits of detection were 1.0 ng/L, 2.5 and 4.5 ng/L for TCC, TCS, and MTCS, respectively. The linearity of the method was observed in the range of 5-2000 ng/L, with correlation coefficients (r2) >.99. The spiked recoveries of TCC, TCS and MTCS in water sampleswereachieved in the range of 89.5% -96.8% with RSD below 5.7%. The proposed method has been successfully applied to analyze real water samples and satisfactory results were achieved.

Synthesis of curcuminoid-imprinted polymers applied to the solidphase extraction of curcuminoids from turmeric samples

A molecular imprinting polymer technique was successfully applied to precipitation polymerization by using styrene as a functional monomer, curcuminoids as templates, acetonitrile as a porogenic solvent,benzoyl peroxide as the initiator, and ethylene glycol dimethacrylate as the crosslinker. The effects of interaction on the adsorption capacity of the molecularly imprinted polymer(MIP) and non-imprinted polymer(NIP) were investigated. A comparison of the adsorption capacity for MIP and NIP indicated that the NIP had the lowest adsorption capacity. The curcuminoid-imprinted polymer(Cur-MIP) was synthesized from 0.0237 mmol of styrene, 47.0 g of acetonitrile, 1.0238 mmol of ethylene glycol dimethacrylate, 0.0325 mmol of curcuminoids, and 0.2480 mmol of benzoyl peroxide. A high-performance liquid chromatography method with fluorescence detection was developed and validated for various chromatographic conditions for the determination of the curcuminoids in turmeric samples. The sample solution was separated using the Cur-MIP via solid-phase extraction and analyzed on a Brownlee analytical C_(18) column(150 mm ×6 mm, 5 mm) using an isocratic elution consisting of acetonitrile and 0.1%trichloroacetic acid(40:60, v/v). The flow rate was maintained at 1.5 m L/min. The fluorescence detector was set to monitor at λex? 426 nm and λem? 539 nm. The quantification limit values were found to be16.66, 66.66, and 33.33 mg/L for curcumin, demethoxycurcumin, and bisdemethoxycurcumin, respectively. Thus, we concluded that the Cur-MIP and high-performance liquid chromatographic-fluorescence method could be applied to selective extraction and could be used as a rapid tool for the determination of curcuminoids in medicinal herbal extracts.

Determination of Trace Amount of Polycyclic Aromatic Hydrocarbons in Urban Sewage by Solid-phase Extraction Coupled with High Performance Liquid Chromatograph

[Method] This study aimed to determine trace amount of polycyclic aromatic hydrocarbons(PAHs) in urban sewage by using solid-phase extraction(SPE) coupled with high performance liquid chromatograph(HPLC).[Method] From the aspects of solid-phase extraction column,elution solvent,elution volume,elution speed and so forth,the test conditions of SPE-HPLC method were optimized,and trace amount of PAHs in urban sewage was determined.[Result] The optimized solid-phase extraction conditions were SUPELCLEAN LC-18 solid-phase extraction column,methylene dichloride as elution solvent,15 ml elution volume,2 ml/min elution speed,5 ml/min loading speed,1 000 ml water with 200 ml methanol loading volume.Under the optimized extraction conditions,the recovery was high,namely 76.3%-105.2%;relative standard deviation was 3.8%-6.0%,showing good precision;detection limit was low,only 0.000 8-0.048 0 μg/L.[Conclusion] This method is user-friendly,with high sensitivity and good precision,and suitable for continuous determination of a large volume of water samples.

Application of Online Solid-phase Extraction Technology in the Field of Environmental Analysis

For purpose of purification and enrichment, environmental samples usually need to be pretreated before analysis because of low concentration of residual organic matters. Solid-phase extraction （SPE） is one of the frequently used methods of pretreatment. This article introduces the methodological principle and flow channel of SPE as well as the categories of frequently used small extraction column, analyzes the application of online SPE technology in environmental analysis, generalizes the advantages of online SPE and sets forth its developmental trend.

基于MSEP@CTAB的磁固相萃取结合HPLC-UV法测定环境水和饮品中的苏丹红

目的制备一种有机/无机双功能化磁性纳米复合材料MSEP@CTAB,将其作为磁固相萃取的吸附剂并结合HPLC-UV法检测环境水和饮品中的苏丹红残留。方法以Fe_(3)O_(4)作为磁性纳米粒子,选择海泡石(Sepiolite,SEP)为无机材料对其进行修饰,再采用十六烷基三甲基溴化铵(cetyltrimethylammonium bromide,CTAB)进行有机改性,得到有机/无机双功能化磁性纳米复合材料MSEP@CTAB;利用傅里叶变换红外光谱仪、透射电子显微镜、X射线衍射仪、振动样品磁力针和全自动比表面及孔隙度分析仪等对复合材料进行表征;考察并优化磁固相萃取条件。结果在最佳实验条件下,3种苏丹红染料在质量浓度0.5~50 ng·mL^(-1)内线性关系良好(R^(2)≥0.9962),检测限为0.05~0.07 ng·mL^(-1),定量限为0.17~0.23 ng·mL^(-1),日内和日间精密度分别为1.8%~8.8%和2.8%~9.0%。该方法被成功应用于环境水和饮品中3种苏丹红染料的检测,加标回收率为82.5%~108.2%。结论所建立的方法简便、快速、灵敏,为环境水和饮品中痕量苏丹红染料的检测提供了一种可行的策略。

固相萃取-HPLC-ESI-MS/MS法测定水中全氟化合物

搭建了固相萃取-超高效液相色谱-电喷雾-串联质谱仪,发现测定水中17种全氟化合物(PFCs)的检测方法。采用玻璃纤维滤膜过滤样品,WAX萃取柱(固相萃取小柱)对样品进行前处理后,柱温和流速分别设定为40℃和0.3 mL/min,使用乙酸铵和乙腈作为流动相,利用梯度洗脱程序进行分离,超高效液相色谱-串联质谱多反应监测(MRM)负离子模式测定,内标法定量。通过优化实验的样品前处理条件和测试参数,标准曲线绘制结果显示,在0~100μg/L范围内,17种全氟化合物线性良好(R大于0.999)。低、中、高3种质量浓度的实际加标样品的相对标准偏差在0.53%~12.00%,回收率在70.7%~114.0%。测试结果表明该方法可以应用于实际检测工作。

HPLC法测定灵芝孢子油中邻苯二甲酸酯类化合物

目的 建立固相萃取(Solid-Phase Extraction,SPE)净化结合HPLC分别测定灵芝孢子油中邻苯二甲酸二(2-乙基)己酯(DEHP)和邻苯二甲酸二正丁酯(DBP)含量的方法。方法 灵芝孢子油经甲醇萃取后使用SPE小柱净化,收集净化液经氮吹浓缩后,采用Supersil ODS_(2)色谱柱(250×4.6 mm,5μm),流动相为甲醇-水(检测DEHP流动相体积比为93∶7,检测DBP流动相体积比为75∶25),流速1.0 mL·min^(-1),柱温40℃,检测波长235 nm,外标法定量。结果 DEHP在0.11~44.52μg·mL^(-1)(r=0.9997)、DBP在0.11~44.28μg·mL^(-1)(r=0.9999)内呈良好的线性关系;DEHP和DBP的加样回收率分别为92.56%~97.55%和90.55%~97.70%。结论 建立的含量测定分析方法快速准确,灵敏度高,重复性和稳定性较好,适用于灵芝孢子油中DEHP和DBP的检测。

SPE-HPLC法检测畜禽养殖废水中四环素残留——基于植物净化系统多介质检测优化

通过对前处理条件进行优化,建立了一套固相萃取(SPE)-高效液相色谱(HPLC)检测多介质中四环素残留量的方法。底泥和植物组织经Na_(2)EDTA-Mcllvaine的甲醇溶液(1∶1,v∶v,pH=4)提取后,分别以HLB小柱(底泥)和SAX/PSA-HLB串联柱(植物组织)富集净化;水样经Na_(2)EDTA溶液(pH=3.4)提取后,以HLB小柱富集净化后再进行HPLC检测。四环素添加浓度为5 mg/L(低浓度)和50 mg/L(高浓度)时,水体、底泥以及植物根系等3种基质中的加标回收率分别达到106.5±1.0%、90.7±8.0%、92.8±1.0%(5 mg/L)和93.9±1.8%、78.5±0.4%、78.8±0.4%(50 mg/L),方法准确度和精密度均较高。四环素在水体、底泥以及植物根系中的检出限分别为3.83μg/L、0.15 mg/kg以及1.53 mg/kg,方法在0~50 mg/L范围内具有良好的定量线性关系。应用该方法检测人工模拟畜禽养殖废水系统各介质样品,检出四环素浓度为nd~655.94μg/L(水体)和0.59~78.45 mg/kg(底泥、植物组织),表明该方法有效可行。

HPLC测定生物样品中头孢克肟含量

建立测定血浆及支气管肺胞灌流液（ＢＡＬ）中头孢克肟（ＣＦＸ）浓度的高效液相色谱方法．用Ｓｅｐ－ＰａｋＣ１８样品预处理小柱富集、分离、纯化生物样品中的ＣＦＸ，在Ｃ１８柱上，以甲醇—水—磷酸盐缓冲液（２２∶２８∶５０，Ｖ／Ｖ）为流动相，检测波长２８６ｎｍ，对头孢克肟进行定量分析．血浆中０．１～４．０ｍｇ／Ｌ、ＢＡＬ中０．０５～１．６ｍｇ／４Ｌ浓度范围内具有良好线性关系，血浆和ＢＡＬ回收率分别为（９９．２±２．３６）％和（９７．９±２．７７）％．血浆及ＢＡＬ的日内、日间ＲＳＤ均小于５％．方法简单、灵敏、准确，特别适用于生物样品中低浓度ＣＦＸ的测定．

HPLC荧光检测法测定新药文拉法辛血浆浓度的方法研究

目的 :建立一种反相高效液相色谱法测定血浆中文拉法辛浓度。方法 :血样经固相萃取 ,以 1%三乙胺 -乙醚洗脱所需组分 ;用ODS柱分析 ,流动相为乙腈 - pH 6 8磷酸盐缓冲液 -三乙胺 (30∶70∶1) ,磷酸调 pH至 2 8;内标为马普替林 ;荧光检测 ,激发波长为 2 76nm ,发射波长为 5 98nm。结果 :文拉法辛的线性范围为 10～ 80 0ng·mL-1;最低检出量为3ng ,最低血药检测浓度为 6ng·mL-1(S/N >3) ;文拉法辛在浓度 10 ,5 0 ,10 0 ,5 0 0ng·mL-1的萃取回收率和方法回收率分别为 98 4%～ 10 2 0 %和 98 2 %～ 10 5 7% ;日内与日间的RSD分别小于 6 %和 9% (n =5 ) ;马普替林的萃取回收率为 81 7%。结论 :本法灵敏 ,简单 ,准确 ,重现性好 ,可满足药动学研究与治疗药物监测的要求。

HPLC法测定犬血浆中葛根素含量

目的:建立血浆中葛根素含量测定方法。方法:色谱柱:Waters Symmetry C18柱(150 mm×3.9 mm,5μm);流动相:乙腈-0.0075 mol·L-1磷酸盐缓冲液(pH 2.7)(10:90);测定波长:248 nm;柱温:40℃;流速:1 mL·min-1。血浆样品采用固相萃取处理。并用健康家犬6只,单剂量给予葛根总黄酮片600 mg,进行了血药浓度测定。结果:血浆样品中葛根素无干扰,最低检测限为0.1 ng·mL-1,葛根素在0.0175-2.2μg·mL-1范围内血浆药物浓度与峰面积线性关系良好,r=0.9995,回收率为85.0%-117.1%,日内、日间RSD分别为7.5%-11.6%和4.7%-8.7%。结论:本法样品处理方法简单,无干扰,提取完全,灵敏度高,重现性好,可用于葛根素生物样本分析。

人血浆中氯氮平及去甲氯氮平的固相萃取HPLC测定

建立了HPLC法测定人血浆中的氯氮平及去甲氯氮平含量。采用C18柱,流动相为甲醇-水-三乙胺-乙酸(600∶400∶4∶2),检测波长254nm,固相萃取法处理血样,地西泮为内标。氯氮平及去甲氯氮平在50～2000ng/ml范围内线性关系良好。平均方法回收率分别为103.1%和102.1%。

离子对SPE-HPLC法检测生物检材中的百草枯

目的建立生物检材中百草枯的简便、快速、灵敏、可靠的高效液相色谱分析方法。方法生物检材酶解后,用以十二烷基三甲基溴化铵和十二烷基硫酸钠预处理过的C18固相柱萃取,HPLC/DAD进行分析。结果回收率81%～94%,检出限为1ng·mL-1,线性范围50ng·mL-1～1mg·mL-1,结论此方法适用于中毒生物检材中百草枯的检测。

传统肉制品中杂环胺的HPLC测定

以烤鸭、烤羊肉、烧鸡、卤牛肉和肉松5种传统肉制品为对象分析其杂环胺含量。样品净化前处理通过串联Ex-trelut-PRS-C18柱进行固相萃取,经TSK-gel ODS-80TM柱分离并以配备二极管阵列和荧光检测器的HPLC对杂环胺进行测定。结果表明,该方法中15种杂环胺的线性范围为0.01-1.00ng·μL-1,检测限为0.5pg·g-1-0.3ng·g-1,回收率为58.60%-98.75%,相对标准偏差为1.81%-8.77%。该方法线性范围广,灵敏度和准确度较高,净化效果好,可满足定量分析的要求。在5种肉制品中检测出6种非极性杂环胺,且不同的肉制品中杂环胺的种类与含量不同。9H-吡啶并[4,3-b]吲哚（Norharman）与1-甲基-9H-吡啶并[4,3-b]吲哚（Harman）均存在于5种肉制品中,含量分别为42.75ng·g-1和33.9ng·g-1。3-氨基-1-甲基-5H-吡啶并[4,3-b]吲哚（Trp-P-2）只存在于烤鸭与烤羊肉中,2-氨基-1-甲基-6-苯基-咪唑并[4,5-b]吡啶（PhIP）在烤鸭、烤羊肉和肉松中检出,而2-氨基-9H-吡啶并[2,3-b]吲哚（AaC）和2-氨基-3-甲基-9H-吡啶并[2,3-b]吲哚（MeAaC）只存在于肉松中,其含量均小于2ng·g-1。

固相萃取HPLC联用法测定食品中丙烯酰胺含量的研究

实验选用C18固相萃取(SPE)柱对样品进行净化,用DIKMA公司C18(150×4.6mm,5μm)钻石柱为色谱柱,以5%甲醇的水溶液为流动相,以197nm为检测波长,对不同食品中的丙烯酰胺进行了分离和检测。结果显示:丙烯酰胺在0.05～10ng范围内呈良好的线性关系,相关系数R2=1,其标准回收率为99.84%±1.55%,变异系数为1.55%。样品中的丙烯酰胺加样回收率分别为92.34%±0.51%,变异系数分别为0.55%。丙烯酰胺的最低检测限是2.5ng/g。该方法样品处理简单,灵敏度高,可在有关实验室推广应用。

基质固相分散萃取-高效液相色谱串联质谱法(HPLC-MS-MS)同时测定茶叶中11种农药的残留量

建立了茶叶中3类11种农药的分散固相萃取-高效液相色谱串联质谱（HPLC-MS-MS）的检测方法。茶叶样品以乙腈-乙酸（体积比99∶1）提取,以PSA为净化剂基质固相分散萃取,然后通过C18色谱柱,以甲醇/水（含甲酸铵）溶液进行梯度洗脱,采用电离喷雾电离方式（ESI＋）,通过多反应监测（MRM）定量。结果表明：11种农药的分析时间约为20 min,在0～500 ng·mL-1范围内线性相关,相关系数大于0.9995,方法检测限为0.1～1.7μg·kg-1。测定了茶叶样品中11种农药的残留量,加标回收率为62.4%～114.8%（添加水平分别为10～400μg·kg-1）,相对标准偏差（RSD）为3.28%～19.34%。选取了5个不同类型的茶叶样品,检测其中11种农药的残留量,检出结果差异较大。其中绿茶中11种农药的检出量为1.7～339.4μg·kg-1,加标回收率为86.1%～104.1%,相对标准偏差（RSD）均小于20%（n=6）。本方法准确、灵敏、简单、快速、安全,能满足茶叶样品中多种农药残留分析的要求。

南海海域软骨藻酸(DA)贝类毒素的HPLC方法检测

采用高效液相色谱法测定南海海域多种水产品中软骨藻酸(DA)的含量。样品粗提液通过LC-SAX强阴离子柱固相萃取净化,在乙腈-0.1%三氟乙酸水溶液(体积比为19:81)流动体系下进行定性分析,以外标法进行定量。结果表明,DA在1 mg/L～25.0 mg/L范围内有良好的线性关系,R=1.0,平均回收率为95.3%;11批次样品中有9批次被检出有DA累积,扇贝和钝齿短桨蟹中的DA累积较高,分别为10.113μg/g和18.202μg/g。

人血浆中阿西美辛及其代谢物吲哚美辛的固相萃取-HPLC-UV法测定

以氟比洛芬为内标 ,采用固相萃取 -紫外检测的 HPL C法同时测定人血浆中阿西美辛和吲哚美辛。灵敏度和选择性均高 ,最低定量限为 2 0 ng/ ml,线性范围为 2 0～ 10 0 0 ng/ ml。