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为实现微量大鼠脑微透析液中3种儿茶酚胺化合物的高灵敏检测,采用d0/d3-10-甲基-吖啶酮-2-磺酰氯(d0/d3-MASC)为同位素编码衍生化试剂,联合使用超声辅助分散液液微萃取技术,建立了超高效液相色谱-串联质谱(UHPLC-MS/MS)快速测定多巴胺(DA)、肾上腺素(EP)和去甲肾上腺素(NE)的分析方法。分别以d0-MASC和d3-MASC衍生微透析液样品和对照品,混合后采用分散液液微萃取技术富集净化,再进行UHPLC-MS/MS检测,以d3-MASC衍生物作为相应d0-MASC衍生物的内标物进行定量。结果表明,在p H 10.8乙腈水溶液中于37℃衍生反应3 min,即可实现待测物的完全分离与检测,3种儿茶酚胺化合物的线性范围为0.02~10.0 nmol/L,相关系数大于0.995,检出限为0.005~0.010 nmol/L,定量下限为0.018~0.040 nmol/L。该方法与已报道方法相比具有显著优势,能够满足大鼠脑微透析液中儿茶酚胺的检测要求。 相似文献
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液相色谱-串联质谱法同时测定血浆中白藜芦醇苷及其代谢产物 总被引:1,自引:0,他引:1
建立同时测定大鼠血浆中白藜芦醇苷及其代谢产物白藜芦醇的液相色谱-串联质谱方法。以Lichro-spher C18色谱柱为分析柱,乙腈-水为流动相,采用电喷雾离子源(ESI),以多反应监测(MRM)模式检测,内标法定量,用于定量分析的离子反应分别为m/z389/227(白藜芦醇苷)和m/z227/143(白藜芦醇)。血浆中的白藜芦醇苷及白藜芦醇用乙酸乙酯提取,N2吹干乙酸乙酯,残留物用甲醇溶解,注入LC/MS/MS系统进行检测。在选定的样品预处理、色谱及质谱条件下,白藜芦醇苷、白藜芦醇及内标物能够达到基线分离而且离子化效果好。用LC/MS/MS法检测大鼠血浆中的白藜芦醇苷及其代谢产物白藜芦醇,线性范围0.4~200μg/L,日内、日间精密度(RSD)均小于15%;检测血浆低、中、高3个浓度(1、20、100μg/L)白藜芦醇苷的回收率分别为106.2%、97.8%和91.6%;检测血浆低、中、高3个浓度(1、20、100μg/L)白藜芦醇的回收率分别为113.2%、103.6%和93.4%。本方法具有灵敏、准确、快速的特点,可用于白藜芦醇苷的药代动力学研究。 相似文献
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建立了水体沉积物中阿维菌素残留的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。沉积物样品采用超声微波萃取、固相萃取净化。待测物通过Thermo-C18色谱柱(50 mm×2.1 mm,1.9μm)分离,乙腈∶乙酸-乙酸铵缓冲液∶水混合溶液(75∶10∶15,体积比)为流动相洗脱,大气压化学电离-多反应负离子监测模式检测,内标法定量。通过加入内标物甲氨基阿维菌素苯甲基盐并采用基质加标标准曲线进行校正。研究表明,阿维菌素的线性范围为1.6~400μg/L,相关系数(r2)达到0.999 3。不同浓度加标样品的相对标准偏差(n=3)为2.2%~16.2%,方法的检出限为0.18 ng/g(干重)。野外样品检测显示,HPLC-MS/MS方法与衍生化-液相色谱/荧光检测法的分析结果相当,但前者更灵敏、简便,适用于沉积物中痕量阿维菌素残留的测定。 相似文献
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建立了在线固相萃取-高效液相色谱-串联质谱法(On-line SPE HPLC-MS/MS)测定大鼠血浆中S/R-阿姆西汀手性异构体的方法。血浆样品经过以下预处理步骤:采用甲醇-乙腈(50∶50,V/V)沉淀蛋白;应用On-line SPE将血浆样品中的其它杂质去除;将保留在SPE柱上的阿姆西汀和内标洗脱后用分析柱进一步分离。分离后再用串联质谱法分别测定大鼠血浆中S/R-阿姆西汀的含量。SPE柱为Retain PEP Javelin(10 mm×2.1 mm);分析柱为ZORBAX SB-C18(50 mm×2.1 mm×3.5μm)。质谱采用电喷雾离子源(ESI),多反应监测(MRM)模式,检测离子为正离子,分别选择m/z 292.1/154.0和260.4/116.2作为S/R-阿姆西汀和内标(普萘洛尔)的检测离子对。结果表明,S/R-阿姆西汀的线性范围为0.2~1000μg/L,相关系数R分别为0.9903和0.9951,批内精密度RSD分别为1.2%~12.0%和0.4%~11.2%,回收率分别为94.2%~101.6%和94.3%~109.4%之间。本方法显著提高了阿姆西汀的检测灵敏度,可以满足大鼠灌胃给予阿姆西汀两种异构体的药代动力学研究要求。 相似文献
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高效液相色谱-二极管阵列检测法及高效液相色谱-电喷雾串联质谱法测定植物源性蛋白中残留的三聚氰胺 总被引:66,自引:7,他引:59
建立了高效液相色谱-二极管阵列检测器(HPLC-DAD)及HPLC-电喷雾串联质谱(ESI-MS/MS)测定植物源性蛋白中残留的三聚氰胺的方法。利用HPLC-DAD进行样品中三聚氰胺的初筛,利用HPLC-MS/MS进行确证。采用三氯乙酸溶液沉淀样品中的蛋白,同时提取目标分析物,质谱检测时样品再经强阳离子固相萃取柱富集净化。HPLC-DAD的检测低限为10 mg/kg,HPLC-MS/MS的检测低限为0.5 mg/kg;HPLC-DA的添加回收率为76%~88%,HPLC-MS/MS的添加回收率为72%~82%(基质匹配曲线校正),两种方法的添加回收率的相对标准偏差(RSD)为3.4%~6.4%。 相似文献
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Guo J Zhao Y Zhao L Zhang W Zhang A Xu B 《Rapid communications in mass spectrometry : RCM》2006,20(11):1701-1708
A quantitative method for the simultaneous determination of CTN986, a flavonol triglycoside, and its two deglycosylation products rutin and hirsutin in rat serum was developed and validated for the investigation of the pharmacokinetics of CTN986. Analytes were isolated from the serum samples (200 microL) prior to analysis by liquid chromatography/tandem mass spectrometry (LC/MS/MS) using C(18) solid-phase extraction, and were separated on a Zorbax C(8) reversed-phase column with an isocratic mobile phase consisting of methanol/isopropanol/water/formic acid (20:10:70:0.1, v/v/v/v). The protonated analytes generated in the positive ion mode were monitored through multiple reaction monitoring in an eletrospray ionization source. Calibration was performed by internal standardization with CTN987, a flavonoid structurally similar to CTN986, and regression curves were constructed ranging from 2 to 1000 ng/mL in 200 microL serum samples. The intra- and inter-day precision values were below 11% and accuracy was between -2.37 and 1.4% for all quality control samples. This quantitation method was successfully applied to pharmacokinetic studies of CTN986 in rats following oral and intravenous administration. Rutin and hirsutin were not detected in rat serum. 相似文献
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超高效液相色谱-串联质谱法快速测定农产品中残留的种衣剂农药 总被引:2,自引:0,他引:2
应用超高效液相色谱-串联质谱(UPLC-MS/MS)联用技术,建立了高灵敏、快速地同时检测农产品中8种种衣剂农药残留量的方法。样品经甲醇-水(体积比为1∶1)提取后,无需经过任何净化过程;以梯度流动相洗脱、经Acquity UPLC C18超高效液相色谱柱分离;电喷雾正离子(ESI+)采集模式、多反应监测模式(MRM)对定量离子和定性离子进行MS/MS测定。8种种衣剂农药在0.001~0.20 mg/L范围内线性关系良好(r≥0.997)。添加浓度为0.006~1.2 mg/kg时,回收率为60%~110%,相对标准偏差小于10%;方法的检出限为0.0005~0.002 mg/kg。该方法仅需约2 min的检测时间,而且灵敏、准确,适合于水果、蔬菜、粮谷等农产品中种衣剂农药残留量的快速、高灵敏地检测分析。 相似文献
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GC-NCI-MS分析茶叶中17种有机氯和拟除虫菊酯农药残留 总被引:17,自引:0,他引:17
建立了茶叶试样中17种农药残留(8种有机氯和9种拟除虫菊酯农药)的气相色谱-负化学离子源-质谱(GC-NCI-MS)联用的分析方法.茶叶试样用V(正己烷)/V(丙酮)=1/1混合提取剂超声提取,经Florisil硅藻土和中性氧化铝混合层析柱净化后,以环氧七氯为内标物,采用GC-NCI-MS的选择离子监测方式(SIM)分析;探讨了茶叶试样的基体诱导色谱响应增强影响所产生的分析误差及其减小的措施,用空白试样基体匹配校准曲线法(MC法)定量分析.当加标质量浓度水平为20,50和200μg/kg时,加标回收率为67.9%~129%,相对标准偏差为1.0%~20%,除氯菊酯农药的检出限为8.3μg/kg外,其余大部分农药的检出限均小于1.0μg/kg,线性范围为10~500μg/kg,相关系数均大于0.996,此方法成功地应用于茶叶试样中痕量农药残留的分析. 相似文献
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A gradient liquid chromatography-tandem mass spectrometry method has been developed and validated for the determination of gastrodin and ligustrazine hydrochloride in rat plasma and brain dialysates. Zolpidem was used as internal standard. For plasma samples, solid-phase extraction was used and the brain dialysates were collected from freely moving rats using brain microdialysis. Both were followed by HPLC separation and positive electrospray ionization tandem mass spectrometry detection (ESI–MS–MS). Chromatographic separation was achieved on a Symmetry RP-18 column using gradient elution with methanol and water containing 0.5% formic acid and 2 mM ammonium formate. Selected reaction monitoring (SRM) mode was used for quantitation. Good linearities were obtained in the range of 0.05–100 and 0.01–50 μg mL?1 for gastrodin and ligustrazine hydrochloride in rat plasma, and 0.05–1,000 ng mL?1 for both in dialysate. The lower limit of quantitation was 0.01 ng mL?1 for gastrodin and 0.05 ng mL?1 for ligustrazine. The method is precise and reliable and can be applied to pharmacokinetic studies. 相似文献
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研究建立了一种加速溶剂萃取-固相萃取/超高效液相色谱-串联质谱法(SPE-UPLC-MS/MS)测定育苗基质中矮壮素和助状素的分析方法。样品采用快速溶剂萃取仪(ASE)提取,经CBA弱阳离子交换柱净化后,在亲水作用色谱柱上用SeQuant ZLC-HILIC MEKCK色谱柱进行分离;电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测。矮壮素和助状素的质量浓度在0.2~10 μg/kg范围内线性关系良好(r2>0999),在2、5、10 μg/kg加标水平的平均回收率分别为77%~106%和97%~111%,相对标准偏差(RSD)分别为7.3%~21.7%和5.6%~16.1%,检出限(LOD)均为0.02 μg/kg,定量下限(LOQ)均为0.1 μg/kg。该方法简便、快速、灵敏、准确,适合育苗基质中矮壮素和助状素残留的确证和定量测定。 相似文献
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Laganá A Fago G Marino A Santarelli D 《Rapid communications in mass spectrometry : RCM》2001,15(4):304-310
An analytical procedure that enables routine analysis for trace determination of six anabolic macrocyclic lactones (zearalenone, alpha- and beta-zearalenol, zearalanone, zeranol, and taleranol) in sewage treatment plant (STP) samples has been developed. The method uses solid-phase extraction, followed by high-performance liquid chromatography with on-line tandem mass spectrometry using atmospheric pressure chemical ionization (LC/APCI-MS/MS). The extraction of these compounds from filtered water samples was performed off-line with C(18) solid-phase cartridges. The detection was achieved by isocratic reversed-phase high-performance liquid chromatography coupled with an heated nebulizer (HN) APCI interface operating in negative ion mode. Mean recovery of the analytes in STP effluent samples generally exceeded 81%. This method was used to determine the occurrence of target analytes in the aquatic environment. In the selected STP effluent samples, zearalenone and alpha-zearalenol were detected in the ng/L range. 相似文献
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Jun Fu Chao Fang Yong‐Yao Cui Li‐Min Yang Liang Zhu Xue‐Mei Feng Pei‐Li Zheng Yang Lu Hong‐Zhuan Chen 《Biomedical chromatography : BMC》2009,23(10):1044-1050
A sensitive, accurate and precise liquid chromatography–tandem mass spectrometry method was developed for the determination of (?)‐satropane (3α‐paramethyl‐benzenesulfonyloxy‐6β‐acetoxy‐tropane) in rabbit aqueous humor. Since (?)‐satropane may be absorbed from the aqueous humour with resultant systemic side effects, the LC‐MS/MS method was also evaluated for its applicability in analyzing plasma samples containing this compound. (?)‐Satropane and phentolamine (the internal standard, represented as IS) were detected by multiple reaction monitoring using the transitions m/z 354–182 and 282–212, respectively. The calibration curve was linear over the ranges 2–500 and 5–1000 ng/mL, and the values of the lower limit of quantification were 2 and 5 ng/mL for the microdialysis dialysate and rat plasma samples, respectively. The intra‐day and inter‐day precision and accuracy were better than 8.6 and 6.00%, respectively, in both matrices investigated. The absolute recovery of the plasma samples was more than 76.30%. The average matrix effects of (?)‐satropane were 91.72 and 83.05% in the microdialysis dialysate and plasma samples, respectively. The validated method was successfully applied to analyze (?)‐satropane in microdialysis dialysate and rat plasma samples, and this assay has been used to quantify (‐)‐satropane in the pharmacokinetic and toxicokinetic studies in our laboratory. Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
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实验采用HCl-HNO3-HF-HClO4混合酸为消解体系对样品进行前处理,加入1.0 mL盐酸羟胺溶液(100 g/L)溶解残渣,选择合适的同位素,以103Rh为内标测定Cr、Co、Ni、Cu、Zn和Cd,以193Ir为内标测定Tl和Pb,建立了电感耦合等离子体质谱(ICP-MS)法测定硅锰冶炼渣中8种重金属元素的方法。实验发现,样品前处理选择HCl∶HNO3∶HF∶HClO4=5∶5∶5∶1,并在复溶阶段加入1.0 mL盐酸羟胺溶液(100 g/L)可以完全消解样品,实验采用KED模式和干扰系数校正法消除质谱干扰,样品中待测元素的测定结果不受基体成分的干扰。通过绘制校准曲线及测定流程空白,各元素校准曲线的相关系数均大于0.9999,方法检出限为0.006~0.19 mg/kg,方法定量限为0.018~0.57 mg/kg。对硅锰渣实际样品进行测定,各元素的相对标准偏差(RSD,n=11)在0.83%~4.1%,加标回收率为94.7%~106%;经过人员比对实验,相对偏差为-4.54%~4.24%。测定结果稳定可靠,能满足硅锰冶炼渣中8种微量金属元素含量的分析检测要求。 相似文献
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Simultaneous determination of cefazolin in rat blood and brain by microdialysis and microbore liquid chromatography 总被引:3,自引:0,他引:3
A sensitive microbore liquid chromatographic method combined with the minimally invasive technique of microdialysis was devised for simultaneously and continuously monitoring the levels of unbound blood and brain cefazolin in rats. Microdialysis probes were inserted into the jugular vein and brain striatum for blood and brain sampling, respectively. Chromatographic conditions consisted of a mobile phase of methanol-acetonitrile-100 mM monosodium phosphoric acid (20:10:70, v/v, pH 4.5) pumped through a microbore reversed-phase column at a flow rate of 0.05 mL/min. The ultraviolet detection wavelength was set at 270 nm. An on-line design allowed direct and continuous analysis of protein-free samples in the dialysate. Microdialysis probes, being home-made, were screened for acceptable in vivo recovery. Chromatographic resolution and detection were validated for response linearity as well as intra-day and inter-day variabilities. This method was then applied to pharmacokinetic profiling of protein unbound cefazolin in both the blood and brain following intravenous administration (10 mg/kg, i.v., n = 6). Rapid appearance of cefazolin in the rat brain striatal dialysate following drug injection suggested good blood-brain barrier penetration. According to a non-compartmental pharmacokinetics model, the area under the concentration (AUC) vs time ratio of cefazolin in rat brain and blood was 6%. 相似文献