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建立了固相萃取-超高效液相色谱(UPLC)同时测定乳制品中苹果酸、酒石酸、乳酸、乙酸、柠檬酸、富马酸等6种有机酸的分析方法。样品用体积分数1%氨水溶液提取,调节至中性后经MAX柱净化,用Acquity UPLC HSS T3色谱柱(2.1 mm×100 mm,1.8μm)分离,以乙腈和0.02 mol/L KH2PO4缓冲溶液(pH 2.0)作为流动相进行梯度洗脱,二极管阵列检测器检测。6种有机酸在其相应范围内(0.05~5000 mg/L)线性关系良好(r2≥0.999),方法的定量限(信噪比为10)为0.05~25.0 mg/kg,3个不同水平的添加浓度回收率为80.1%~103.2%,相对标准偏差(n=8)在1.9%~11%之间。方法适合于乳制品中6种有机酸的同时检测。 相似文献
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超高效液相色谱-串联质谱法同时测定蜂蜜中硝基咪唑类、磺胺类、喹诺酮类兽药残留 总被引:5,自引:0,他引:5
建立蜂蜜样品中硝基咪唑类、磺胺类、喹诺酮类共36种兽药残留的固相萃取-超高效液相色谱-串联质谱检测方法。蜂蜜样品用H3PO4溶液(体积分数0.1%)溶解后,过滤,用Oasis HLB和PSA固相萃取柱净化,外标法定量。测定时用Eclipse Plus C18色谱柱(100 mm×2.1 mm,1.8μm)分离,乙腈-甲醇-甲酸溶液梯度洗脱,质谱测定采用多反应监测(MRM)模式。36种兽药的检出限在0.4~4.0 ng/mL,回收率在63.2%~125.5%,相对标准偏差均低于22%。 相似文献
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利用丙酮-乙腈-正庚烷-磷酸盐溶液提取家兔血浆中游离棉酚,建立家兔血浆中棉酚的高效液相色谱测定方法。色谱柱为ODS-C18(4.6mm×200mm,5μm)柱,流动相为V(甲醇)∶V(1%H3PO4溶液)=85∶15,流速1.0mL/min,检测波长235nm。棉酚在0.66~3.30μg/mL质量浓度范围内峰面积与其浓度间呈现良好的线性关系,r=0.9994;平均加样回收率为95.7%~96.3%;日内、日间RSD分别为0.7%~1.4%和3.7%~7.4%。可用于棉酚生物样品分析。 相似文献
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用高效液相色谱法同时测定虎杖中白藜芦醇、白藜芦醇苷和游离大黄素含量.色谱柱为Waters Symmetry C18柱(3.9 mm×150 mm,5μm),流动相为0.015 mol-1 H3PO4-甲醇,流速为0.5 mL·min-1,检测波长为284nm.样品采用乙醇-水(1 1)溶液和乙酸乙酯提取.江西产虎杖样品中白藜芦醇、白藜芦醇苷和游离大黄素的回收率分别为97.9%,96.1%,95.6%,相对标准偏差小于5%. 相似文献
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烟草中挥发性和非挥发性有机酸的快速测定 总被引:4,自引:0,他引:4
建立了气相色谱-质谱(GC-MS)法快速测定烟草中22种非挥发性、挥发性有机酸的分析方法。采用对甲苯磺酸-硫酸-甲醇(PTSA/H2SO4/CH3OH)酯化试剂对烟草样品进行一次酯化,生成的有机酸酯用GC-MS进行分析。结果表明,酯化时间从20 h缩短到1 h,非挥发酸回收率在93.4%~103.2%之间,相对标准偏差(RSD)小于4.2%;挥发性有机酸回收率在89.2%~99.1%之间,RSD小于3.5%。该方法具有简便、快速,结果准确等特点,用于测定部分烟草样品的挥发性、非挥发性有机酸,取得了满意的结果。 相似文献
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《化学分析计量》2015,(4)
建立离子色谱梯度淋洗抑制电导法测定电厂水中有机酸和无机阴离子的方法。选用Ion Pac AG11–HC(50 mm×4 mm)阴离子保护柱和Ion Pac AS11–HC(250 mm×4 mm)阴离子分析柱对样品进行分离,以氢氧化钾溶液梯度淋洗,自再生抑制电导检测器检测,同时测定电厂水中的有机酸和无机阴离子。F–,Cl–,NO2–,Br–,NO3–的线性范围为0.005~2 mg/L,CH3COO–,HCOO–,SO42–,PO43–的线性范围为0.01~5 mg/L,各组分线性相关系数为0.998 9~0.999 3,检出限为0.122~0.989 ng/m L,测定结果的相对标准偏差小于2.0%(n=7),样品加标平均回收率为97.9%~101.7%。该方法操作简便,实用性强,可以用于电厂水中有机酸和无机阴离子的检测。 相似文献
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应用毛细管气相色谱-质谱轮廓分析方法,测定了33例2.5~4.5岁健康儿童尿中有机酸种类及含量和8例拟诊为苯丙酮尿症儿童尿中的有机酸,结果表明患儿尿样中苯丙酮酸、苯乙酸、邻羟基苯乙酸、对羟基苯乙酸高于正常值10~470倍。为苯丙酮尿症的确诊提供了可靠方法。 相似文献
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A review of sample preparation methods for organic acids in biological fluids, in particular serum and urine, is presented. It covers techniques on organic acid determination without sample preparation, release of organic acids from binding locations, removal of proteins by protein precipitation and ultrafiltration, isolation of the organic acids by liquid-liquid and liquid-solid extraction, purification of the extract, derivatization and pre-fractionation. The various alternative sample preparation steps are compared and critically discussed. Examples of applications including profile analysis of organic acids by gas chromatography (GC), determination of particular organic acids by GC or liquid chromatography and determination of fatty acids as a distinct chemical class of acids demonstrate that the kind of sample preparation chosen depends strongly on the analytical aims. 相似文献
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建立了阀切换-离子色谱法测定1,2-环氧丁烷(1,2-BO)产品中有机酸(甲酸、乙酸和丙酸)的方法。样品经乙醇稀释后,通过阀切换技术,有机酸被IonPac TAC-ULP1捕集柱捕集,然后进入IonPac AS11分析柱分离,并由电导检测器检测。结果表明:甲酸、乙酸和丙酸均能实现较好地分离,在各自的范围内其色谱峰面积呈现良好的线性关系。实际样品的加标回收率为92.5%~111.8%,相对标准偏差小于5.6%(n=3),检出限为0.60~4.80 μg/L。该方法具有前处理简单、快速、准确等特点,适用于不溶于水的有机体系中有机酸的分析。 相似文献
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建立了水样中甲酸、乙酸、丙烯酸和甲基丙烯酸的离子色谱测定方法,采用IonPac AS11-HC阴离子分离柱,以KOH为淋洗液,采用浓度梯度洗脱,可同时测定上述4种有机酸。方法对实际水样中甲酸、乙酸、丙烯酸和甲基丙烯酸的平均加标回收率在80.2%~103.3%,相对标准偏差在5.8%之内,检出限分别为:0.005,0.003,0.005和0.004mg/L;定量下限分别为:0.020,0.012,0.020和0.016mg/L。方法准确、简便、环保,能够满足实际水样的测定需要,且水样中常见的阴离子不会对目标污染物的测定产生影响。 相似文献
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Wei W Wei Z Wang Y Baker AJ Zhao H Li H Hu F 《Journal of chromatographic science》2010,48(10):840-847
An analytical approach based on solid-phase extraction (SPE) with nanosized hydroxyapatite and reversed-phase high performance liquid chromatography (RP-HPLC) for the simultaneous determination of organic acids (oxalic, malic, malonic, citric, and fumaric) and nitrate in xylem saps of the hyperaccumulator Alyssum murale is presented in this study. The optimum experimental conditions for the separation and determination of organic acids and nitrate are studied. The interference from nitrate on oxalic acid in RP-HPLC is eliminated by SPE with nanosized hydroxyapatite, and the simultaneous determination of organic acids and nitrate is achieved by RP-HPLC at the optimum chromatographic conditions. The accuracy of the method is confirmed with an average recovery ranging between 95.2% and 99.8%, the relative standard deviations (RSD) are less than 2.0%. This method is successfully applied to determine the organic acids and nitrate in xylem saps of the hyperaccumulator Alyssum murale. 相似文献
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This paper describes the use of graphene oxide/silica modified with nitro‐substituted tris(indolyl)methane as a solid‐phase extraction sorbent for the determination of organic acids. The resultant graphene oxide/silica modified with nitro‐substituted tris(indolyl)methane was characterized by FTIR spectroscopy and adsorption experiments. Solid‐phase extraction parameters such as sorbent type, sample solution pH, sample loading rate, eluent salt concentration, eluent methanol concentration, elution rate, sample loading, and elution volume were optimized. The method showed good precision, accuracy, sensitivity, and linear response for organic acids analysis over a concentration range of 1–100 μg/L for benzoic acid, p‐methoxybenzoic acid, and salicylic acid and 5–100 μg/L for the remaining organic acids (cinnamic acid, p‐chlorobenzoic acid, and p‐bromobenzoic acid) with coefficients of determination (r2) of higher than 0.9957. Limits of detection from 0.50 to 1.0 μg/L for six organic acids were achieved. The developed method was successfully applied to determine organic acids in real samples. 相似文献
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建立了固相萃取-高效液相色谱(SPE-HPLC)同时测定蜂蜜中5种有机酸(L-苹果酸、马来酸、琥珀酸、柠檬酸、D-苹果酸)含量的方法。蜂蜜经制样后过Bond Elutes SAX固相萃取(SPE)小柱净化,用C18-MS-II反相色谱柱(250 mm×4.6 mm, 5 μm)进行分离,流动相为2%偏磷酸溶液,流速为0.7 mL/min,检测波长为210 nm。在此条件下5种有机酸在相应的线性范围内其线性相关系数均大于0.9967;方法的回收率为86.0%~103.9%,相对标准偏差为5.7%~9.8%(n=6),检出限为0.06~9.4 mg/kg。所建立的方法可用于蜂蜜样品中有机酸的测定。 相似文献
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In this work, a novel technique of aqueous-phase derivatization followed by headspace solid-phase microextraction and gas chromatography-mass spectrometry was developed for the determination of organic acids in urine. The analytical procedure involves derivatization of organic acids to their ethyl esters with diethyl sulfate, headspace sampling, and GC/MS analysis. The proposed method was applied to the determination of methylmalonic acid and glutaric acid in urine. The experimental parameters and method validation were studied. Optimal conditions were obtained: PDMS fiber, extraction temperature 55 degrees C, extraction time 30 min, and 60 microL of diethyl sulfate as derivatization reagent with 2 mg of the ion pairing agent tetrabutylammonium hydrogensulfate. The method was linear over three orders of magnitude, and detection limits were 21 nM for methylmalonic acid and 34 nM for glutaric acid, respectively. Consequently, in-situ derivatization/HS-SPME/GC/MS is an alternative and powerful method for determination of organic acids as biomarkers in biological fluids. 相似文献
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高效液相色谱法测定克鲁维酵母菊芋发酵液中的乙醇,糖和有机酸类代谢成分 总被引:4,自引:1,他引:3
建立了高效液相色谱法同时分析菊芋发酵液中的乙醇和有机酸的方法.采用HPLC有机酸分析柱, 流动相为0.01 mol/L H2SO4,流速为0.5 mL/min, 以紫外和示差折光检测器作为双通道检测手段,同时对克鲁维酵母菊芋发酵液中的柠檬酸、α-酮戊二酸、葡萄糖、丙酮酸、果糖、琥珀酸、乳酸、甘油、乙酸、乙醇进行了定量分析,本方法的回收率为95.8%~109.6%;RSD为0.33%~4.0%,结果表明,本方法简单、快速、准确,适用于监控克鲁维酵母发酵产物并指导整个发酵过程条件的优化. 相似文献