中空纤维三液相微萃取-高效液相色谱法测定水样中吡虫啉

将聚偏氟乙烯（PVDF）中空纤维三液相微萃取与高效液相色谱法联用,建立了分离富集测定水样中吡虫啉的新方法．对聚偏氟乙烯中空纤维的种类、萃取剂、萃取时间等实验参数进行了优化,确立了以磷酸二氢钾溶液为接受相、聚偏氟乙烯中空纤维和正辛醇为介质的三液相微萃取,最佳条件下富集20mL样品溶液,用高效液相色谱法测定,吡虫啉的检测限为0．4ng·mL^-1,吡虫啉的富集倍数为22．75倍．该方法可用于水样中痕量吡虫啉的测定．     

贝类产品中软骨藻酸的HPLC检测方法

建立了高效液相色谱测定贝类产品中软骨藻酸的检测方法,具体过程为:样品先经甲醇浸提后,再用甲醇-水(V（甲醇）∶V（水）=1∶1）提取2次,合并提取液后用Zorbax SB300-C18柱(2.1 mm×250 mm,5 μm)进行分离,以乙腈-0.2%磷酸水溶液（含0.1%三乙胺）（V（乙腈）∶V（磷酸水溶液）=12∶88）为流动相于室温下等度洗脱,流速为0.25 mL/min,进样量20 μL,检测波长为242 nm.结果表明,在建立的提取方法和色谱条件下,软骨藻酸从复杂的样品基体中被分离出来,在0.02~1.0 mg/L质量浓度范围内具有良好的线性关系（r＞0.999）,样品的平均加标回收率为108%,测量方法的RSD为3.5%（n=6）,检出限为23.5 ng/g.所建立的检测方法可适用于对贝类产品中软骨藻酸的快速检测.     

ASE萃取-GPC净化-GC／ECD测定小麦中有机氯农残和多氯联苯

建立了加速溶剂萃取、全自动在线凝胶渗透色谱-浓缩联用系统和氟罗里硅土柱前处理、GC／ECD测定小麦样品中7种多氯联苯(PCBs)和7种有机氯农药(OCPs)的分析方法,并优化了加速溶剂萃取、凝胶渗透色谱净化、GC／ECD的分析条件。结果表明,该方法的样品加标回收率和相对标准偏差分别为:多氯联苯69.8％～87.4％、1.48％～11.0％;有机氯农药70.4％～113.9％、3.54％～17.0％。方法检测限为0.03～0.29μg／kg。用该方法测得小麦样品中7种PCBs质量分数范围为0～157.9μg／kg;7种OCPs质量分数在2.38～10.02μg／kg范围内。该方法快速、灵敏、准确,并且在一个流程中可以同时测定小麦样品中多氯联苯和有机氯农残,适合于大批量样品的测定。     

鸡血藤药材中原儿茶酸的含量测定

建立测定鸡血藤药材中原儿茶酸含量的方法,并对制备供试品溶液的提取溶剂、提取方法、提取次数、药材粒度等进行了考察优化。采用高效液相色谱法,色谱柱:Diamonsil C18色谱柱(250×4.6 mm,5μm);流动相为乙腈-φ=0.5%醋酸水(体积比为10∶90);流速为1.0 mL·min-1;检测波长为260 nm。优化所得供试品溶液的制备方法,药材加水回流提取3次,每次1.5 h,合并提取液并浓缩至小体积,用乙酸乙酯萃取4次,合并乙酸乙酯萃取液,浓缩后的残渣用甲醇-水(体积比为1∶1)溶解并定容,即得。经系统的方法学考察,所建立的方法在原儿茶酸浓度为8.56~214μg·mL-1范围内线性良好(R2=0.999 7),平均加样回收率为99.2%,RSD为2.8%,市售7个批次鸡血藤药材中原儿茶酸的含量为65.81~122.35μg·g-1。该方法准确,重复性好,可用于鸡血藤药材的质量控制。     

基于新型固相萃取-高效液相色谱法灵敏测定牛奶中的药物残留

利用水热法制备了还原氧化石墨烯-硅胶复合物,将其用于固相萃取柱制备,并与高效液相色谱相结合,建立了牛奶中磺胺类药物测定的新方法.对萃取条件进行了优化,优化条件为:0.1 mL的甲醇-乙酸(V∶V′=1∶1.5)混合液为洗脱剂,75mL的样品溶液.在优化条件下,目标物的线性范围为0.1~100μg/L,检出限为0.027~0.078μg/L(RSN=3).新方法用于牛奶样品分析,加标回收率为88.3%~113.6%.     

酱油渣中大豆异黄酮动态逆流提取及分离纯化的研究

以酱油渣干粉为原料,对大豆异黄酮提取条件和纯化方法进行研究.采用实验室模拟动态逆流提取酱油渣中异黄酮,并通过正交设计对大豆类黄酮提取条件进行了优化,确定了大豆类黄酮的最佳提取条件为80%乙醇, 提取前的浸泡时间12h,料液比1:10,得到总异黄酮提取率达0.35%,粗提物的纯度为2.01%.选取3种极性不同的大孔树脂填装制备柱,并利用中低压色谱对大豆异黄酮样品进行纯化.结果表明,NKA9大孔树脂对总大豆异黄酮的纯化效果最好,在60%乙醇洗脱时,产品纯度可达到32%.该方法能实施在短时间内对大豆异黄酮样品进行大量的纯化,满足大豆异黄酮产品生产的需要.     

头发中内源性氢化可的松的高效液相色谱/串联质谱检测

基于高效液相色谱/串联质谱(HPLC/MS/MS)建立了一种检测头发中内源性氢化可的松含量的方法,并与高效液相色谱/荧光法(HPLC/FLU)的测定结果进行比较.头发样品(50 mg)经过清洗与研磨、甲醇提取和C18固相萃取后,在电喷雾(ESI)负离子模式和多反应监测(MRM)方式下进行定性,以外标法进行定量.方法的定...     

鸡蛋中罗硝唑、甲硝哒唑、迪美唑的分析

目的研究测定鸡蛋中罗硝唑、甲硝哒唑、迪美唑方法。方法采用高效液相色谱-质谱联用技术。结果试样在用乙腈进行简单萃取和有机溶剂蒸发后,过滤萃取物,并将所得产物直接注入C18柱的LC-MS-MS系统。其中,母系离子[M H] 由正极气体电离源分裂氩气产生。监测极限、回收率、线性相关性、重现性等有效参数都得以测定。结论方法具有相对快速、灵敏和良好选择性的特点。由于使用了多重控制转移的方法,对试样进行的前处理简单及具有高度的专一性。     

An Automatic Solid Phase Extraction and Ultra-Performance Liquid Chromatography Tandem Mass Spectrometry for Determination of Seven Microcystins at Ultra-Trace Levels in Surface Water

A method was developed for the detection of seven microcystins(microcystin-LR, RR, YR, LA, LY, LW and LF) in surface water using automatic solid-phase extraction(A-SPE) coupled with ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS). The automated solid-phase extraction system was used to extract microcystins(MCs) from water samples. UPLC-MS/MS was used to determine MCs concentrations in just 5 min. Method detection limits were from 0.3 to 0.9 ng/L, microcystin recoveries ranged from 83.8% to 114%, and the relative standard deviation(RSD) varied from 5.6% to 12.5%. This analytical approach was found to be simple, highly sensitive, accurate, which required little manual operation. Additionally, to validate this analytical method, A-SPE+UPLC-MS/MS was applied to characterize the concentration of MCs in Taihu Lake, Wuxi, China.     

基于萃取和超高效液相色谱-串联质谱法的贝类抗生素快速测定方法

建立一种简单、快速的超声波萃取–固相萃取净化–超高效液相色谱串联质谱分析方法, 可以同时测定淡水贝类软组织中磺胺类、喹诺酮类、大环内酯类、β-内酰胺类和氨基糖苷类中15种抗生素。采取超声波萃取法, 对贝类体内的抗生素进行萃取, 用固相萃取方法净化提取液, 最后用超高效液相色谱–三重四级杆质谱对目标物进行分析检测。主要比较两种固相萃取柱Oasis HLB和Oasis PRiME HLB对污染物的净化效率, 后者展现出较好的结果。15种抗生素加标回收率实验结果表明: 当加标浓度为50 ng/g时, 回收率为64%~121%, 相对标准偏差为0.5%~19% (n=3); 添加高浓度(100 ng/g)样品时, 回收率为67%~117%, 相对标准偏差为1%~9%(n=3)。方法检测限(LOD)为0.004~0.5 ng/g (干重), 定量限(LOQ)为0.013~1.67 ng/g (干重)。该方法具有回收率高、检测限低的特点。使用该方法对鄱阳湖3个采样点三角帆蚌中的抗生素进行分析, 结果显示, 在15种抗生素中, 有9种均不同程度地检出, 检出频率和浓度最高的是甲氧苄胺嘧啶, 最高浓度达到78.8 ng/g, 其次是奇霉素(41.2 ng/g)和环丙沙星(39.8 ng/g)。     

Time-resolved fluoroimmunoassay for quantitative determination of tylosin and tilmicosin in edible animal tissues

To quantitatively determine tylosin and tilmicosin in edible animal tissues,a time-resolved fluoroimmunoassay(TRFIA) has been developed and validated.For this purpose,desmycosin-O-carboxymethoxylamine-BSA was fixed onto microtiter plates,standards and samples were loaded and,finally,diluted europium-labeled anti-tylosin antibodies were added.Results show that the limit of detection for tylosin was 0.03 ng mL-1 and that for tilmicosin was 0.05 ng mL-1.The recoveries were 73.6% to 120.5%,with coefficients of variation below 15.6% in various biological matrices spiked with tylosin and tilmicosin at concentrations of 50-200 ngg-1.There was good correlation(R2>0.99) between the TRFIA,an enzyme-linked immunosorbent assay and high performance liquid chromatography data.In conclusion,the new TRFIA is applicable to the detection of tylosin and tilmicosin and is an effective and economical method that will enable high-throughput sample screening.The method is expected to be widely applicable.     

邻苯二甲酸二甲酯印迹聚合物的制备及其在固相萃取中的应用

制备了对增塑剂邻苯二甲酸二甲酯(DMP)具有特异选择性的印迹聚合物(MIP)并成功用于水样中DMP的固相萃取.改变功能单体和聚合方法制备了4种DMP印迹聚合物,并用平衡吸附方法研究了各聚合物对DMP及结构类似物的吸附选择性.进一步将优化聚合物MIP3用作固相萃取(SPE)柱填料,结合气相色谱-质谱联用仪(GC-MS)研究其对某环境水样中DMP的萃取能力.结果表明,MIP3可选择性富集水样中的DMP和净化干扰物质.萃取后DMP的质量浓度由8.2μg/L浓缩至80.06μg/L,富集倍数达到了9.76.回收率为99.16%～103.97%,而传统的液液萃取回收率仅为87.73%～96.14%,方法的灵敏度大大提高,检出限由0.04μg/L降低至0.007μg/L.     

海带中脱落酸的分离纯化及高效液相色谱分析

探索了海带（Laminaria japonica）脱落酸的分离纯化条件,获得最适分离纯化方法为：常温组织匀浆,80%甲醇溶液浸提,乙酸乙酯萃取,硅胶脱色和纯化.在此基础上,利用反向高效液相色谱的方法对样品进行定性定量分析,结果表明样品中含有脱落酸,含量为30.5-60.5μg/kg.这为海藻脱落酸的分离纯化及其活性研究奠定了基础.     

动态微波辅助萃取与高效液相色谱联用测定金银花中的绿原酸

通过流动注射的方法将动态微波辅助萃取与高效液相色谱相连接, 用于测定金银花中的绿原酸. 萃取过程在一个循环体系中完成, 萃取后, 通过采样环采集到的20 μL样品被流动相载带到色谱系统进行分离检测. 在最佳实验条件下得到的检出限和测定下限分别为0.25和0.83 μg/mL, 日内和日间精密度(RSD)分别为3.4%和4.1%, 平均加标回收率为98.1%.     

GCC box in<Emphasis Type="Italic">Arabidopsis PDF1.2</Emphasis> promoter is an essential and sufficient cis-acting element in response to MeJA treatment

The expression of Arabidopsis PDF1.2 gene isregulated by jasmonic acid (JA) and ethylene (ET). It also has been well documented that GCC box is an element responsive to ET, however, the responsive mechanism of JA in such plant defense gene expression is unclear. In this paper, the authors define the essential cis-acting element in PDF1.2 promoter responsive to methyl jasmonate (MeJA) through fragment deletions and site-directed mutageneses combiningAgrobacterium-mediated transient reporter gene expression in tobacco leaves. Firstly, the MeJA inducible expression o fPDF1.2 was confirmed by using the upstream -1.86 kb fragment of PDFI.2 gene. Secondly, the upstream -300— -243 bp fragment of the promoter was evidenced to respond to MeJA. To further characterize this promoter region, three point mutations were introduced into the -300— -243 bp fragment of the promoter. This result showed that the mutation of GCC box abolished MeJA induction, whereas the mutations of the G box-like and the imperfect palindrome sequence did not significantly decrease MeJA inducible effect, indicating that GCC box in PDFI.2 is essential for MeJA induction. The sufficient responsiveness to MeJA of this GCC box was further investigated by 4xGCC fused upstream to the CaMV 35S minimal promoter. This result suggested that the fused promoter was able to activate reporter gene expression in response to MeJA. Thus these results indicate that the GCC box in PDFI.2 is an essential and sufficient element to confer MeJA induction.     

制备高效液相色谱分离纯化系统的研制与开发

介绍一种基于柱层析技术、高效液相色谱技术于一体的计算机智能控制全自动、高性能的化学物质纯化系统。该系统属于高压制备高效液相色谱,采用模块化设计模式,各模块经由计算机工作站软件统一协调,实现进样、分离、馏分收集自动化。该系统应用于中药复杂成分分离、提取和纯化的效率高、馏分损失少、样品回收率高。     

Study on the flow injection micro-column pre-separation system coupled with high performance liquid chromatography for the determination of ecdysterone in traditional Chinese medicine

A flow injection (FI) micro-column system coupled with high performance liquid chromatography (HPLC) was proposed for the pre-separation and determination of active organic component (ecdysterone) in traditional Chinese medicine, Loulu. The factors influencing separation performance were investigated and optimized. Under the optimal conditions, the contents of ecdysterone in Loulu were determined by HPLC system using MeOH-H₂O (40∶60,V/V) as the mobile phase at a flow rate of 1.0 mL/min. The calibration curve was linear in the range of 0.5∼100 mg/L of ecdysterone concentrations. The detection limit of the analyte was 0.11 μmol/L (3σ) with a precision of 0.38% RSD (n=7,c=10.0 mg/L). The average recovery of the method was 98.7%. The proposed method has been applied to determine ecdysterone in practical samples, and the determined values by both external standard method and standard addition method were in good agreement. Compared to the traditional solid extraction method, the system proposed has the advantages of simple procedure, good reproducibility, minimum volume requirement, reduction of matrix interference and low contamination risk. Foundation item: Supported by Education Ministy Foundation for Chinese Returned Scholars and Nature Science Foundation of Hubei province (98J054). Biography: SHUAI Qin (1963-), famale, Ph.D. Candidate.     

高效液相色谱法测定酱腌菜中6种对羟基苯甲酸酯

建立了一种高效液相色谱法同时测定酱腌菜中6种对羟基苯甲酸酯(对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸异丙酯、对羟基苯甲酸丙酯、对羟基苯甲酸异丁酯、对羟基苯甲酸丁酯)含量的检测方法。样品用乙醇水溶液提取,经Oasis HLB固相萃取柱净化,甲醇定容后,紫外检测器于波长为258 nm的条件下测定。6种对羟基苯甲酸酯在0.1～50.0 mg/L范围内呈良好的线性关系,检出限分别为0.1 mg/kg、0.1 mg/kg、0.1 mg/kg、0.1 mg/kg、0.2 mg/kg、0.2 mg/kg(S/N≧3),添加平均回收率85%～110%,RSD<10%。该方法灵敏度高,选择性好,回收率高,简单快捷,能满足常规检测及酱腌菜安全控制的需要。     

催化H2O2氧化吖啶黄固体基质室温磷光法测定痕量秋水仙碱

基于秋水仙碱(COL)能催化过氧化氢(H_2O_2)氧化吖啶黄(AY)的反应,导致AY的室温磷光信号(RTP)剧烈猝灭,据此建立了超灵敏催化H2O2氧化AY固体基质室温磷光法(SS-RTP)测定COL的新方法。此方法的量化限(LOQ)为0.12 fg/斑(对应浓度为3.1×10–13 g·m L–1),灵敏度高、简便、快捷、准确。用于血清中COL的测定,结果与UPLC-MS/MS相吻合。同时测定了动力学常数,其活化能(E)为40.53 k J·mol~(–1),速度反应常数(k)为3.97×10~(–4)·s~(–1)。     

离子液体双水相萃取测定卷烟烟气中酚类物质的研究

建立了卷烟烟气中邻-苯二酚、间-苯二酚、对-苯二酚、苯酚、邻-甲酚、间-甲酚和对-甲酚几种酚类物质的高效液相色谱检测方法.用25%的乙醇水溶液对卷烟样品进行超声提取,再经离子液体双水相分离富集,用高效液相色谱二极管阵列检测器(HPLC-FLD)测定.该方法的富集倍数可以达到20倍,整个操作过程在常温下进行,时间不超过15 min.实验结果表明,在0.02～20 ng/L范围内,几种酚类物质的峰面积均与其质量浓度呈线性相关,R2≥0.999 6,检出限分别为0.06,5.2,1.2,5.3,0.03,0.04 ng/L,相对标准偏差为1.4%～4.6%,回收率为85.1%～96.9%.该方法具有良好的重现性、精密度和更低的检测限.