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建立了丹磺酰氯柱前衍生/高效液相色谱测定牙膏中氨甲环酸(TA)的方法。牙膏经甲醇提取、氮吹至干,再用丹磺酰氯进行衍生。衍生物通过X-Bridge C18色谱柱(250 mm×4.6 mm×5μm)分离,以乙腈和0.1%甲酸水溶液为流动相梯度洗脱,在紫外波长250 nm条件下进行定量测定。系统考察了缓冲溶液p H值、衍生温度和衍生时间对氨甲环酸衍生效率的影响。结果表明,在优化实验条件下,氨甲环酸衍生物与基体杂质达到有效分离,在1~425 mg/L范围内线性关系良好,相关系数为0.999 5;在20,200,1 600 mg/kg 3个加标浓度下的回收率为98.7%~102%,相对标准偏差为0.85%~2.5%,方法检出限为2.0 mg/kg。该方法准确、可靠、灵敏度高,适用于各类牙膏中氨甲环酸的测定。 相似文献
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以甲醇或甲醇与水作流动相,ODS为固定相,测定环己酮的多种过氧化物。平均回收率100.2%~101.6%,测定的相对标准偏差为1.02%~2.51%。 相似文献
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《Analytical letters》2012,45(13):2148-2155
A new method for phytochelatins by high-performance liquid chromatography (HPLC) was developed based on a condensation reaction with monobromobimane to produce fluorescent derivatives. Glutathione, H-(γ-glutamic acid-cysteine)2-glycine-OH, H-(γ-glutamic acid-cysteine)3-glycine-OH, H-(γ-glutamic acid-cysteine)4-glycine-OH, H-(γ-glutamic acid-cysteine)5-glycine-OH, and H-(γ-glutamic acid-cysteine)6-glycine-OH were well separated, with retention times between 14.68 and 22.0 min. The HPLC method had good linearity (r < 0.9991) between 0.1 mg L?1 and 100 mg L?1. The limits of quantification for the analytes (S/N = 3) were 0.08, 0.3, 0.05, 0.3, 0.5, and 0.8 mg L?1, respectively. The recoveries were between 83.0% and 101.33% with relative standard deviations less than 2%. The reported method is simple, accurate, and suitable for the determination of phytochelatins. 相似文献
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高效液相色谱法测定血清中茶碱浓度 总被引:2,自引:0,他引:2
采用高效液相色谱,分析柱:3μm,3.3cm*4.6mm,I.D(Perkin Elmer,USA);预柱:10μm,1cm*2.1mm,I.D(Perkin ELmer,USA);以乙酰氨基酚为内标对氯仿-异丙醇(95:5,V/V)提取样品进行了分析,流动相:0.1mol/L醋酸缓冲液(PH=4.5)-甲醇(70:30,V/V);检测波长:270nm;流速0.5mL/min,3min即完成一次茶 相似文献
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建立了测定肉制品中甘草抗氧化物含量的方法。样品经流动相提取,采用C.8色谱柱分离,以甲醇-0.2mol/L乙酸铵-冰乙酸(体积比70:29:1)为流动相,流速为1.0mL/min,波长为250nm,以保留时间进行定性,峰面积进行定量。甘草酸在1.0-80.0μg/mL范围内线性关系良好,回归方程为y=8.55×10^-5x-0.599(r=0.9997),检出限为1.0mg/kg,定量限为3.0mg/kg,加标回收率为95.7%-103.4%,测定结果的相对标准偏差为1.57%-3.53%(n=6)。该方法适用于检验机构日常检验中大批量肉制品中甘草抗氧化物含量的测定。 相似文献
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《液相色谱法及相关技术杂志》2012,35(8):1491-1497
Abstract A new, sensitive and rapid method for the determination of naloxone hydrochloride as drug in dosage entity and form using HPLC has been developed. Authentic naloxone hydrochloride was used to establish a calibration curve. A linear relationship was obtained for concentrations ranging from 10 μg/ml to 50 μg/ml. The column used was C18, Micropak MCH-10 (monomeric) and the mobile phase was acetonitrile : 0.01 M KH2PO4 (70 : 30) at a flow rate of 2 ml/min. Retention time for naloxone hydrochloride was 3.3 minutes. The proposed method has been proved accurate and precise compared to other pharmacopoeia methods of assay for naloxone hydrochloride. 相似文献
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建立了高效液相色谱(HPLC)-串联紫外检测法检测有机肥中洛克沙胂的分析方法。选用20g·L-1K2HPO4作为提取剂,于60℃温度下超声提取有机肥中的洛克沙胂,采用MAX固相萃取柱净化。结果表明,采用Symmetry ShieldTMRP 18色谱柱,以含0.1%甲酸的0.05mol·L-1 KH2PO4∶甲醇=95∶5(V/V)溶液作流动相,等度洗脱,紫外266nm检测,洛克沙胂的保留时间短,且可完全避开杂质峰的干扰;其平均加标回收率介于81.14%~82.75%之间,相对标准偏差(RSD)7.0%,检出限为20μg·L-1。方法重现性好,精密度高,操作简便,适用于有机肥中洛克沙胂检测。 相似文献
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Simultaneous Determination of Pioglitazone and Glimepiride by High-Performance Liquid Chromatography
A rapid and accurate HPLC method has been developed for simultaneous determination of pioglitazone and glimepiride. Chromatographic separation of the two pharmaceuticals was performed on a Cosmosil C18 column (150 mm × 4.6 mm, 5 m) with a 45:35:20 (v/v) mixture of 0.01 m triammonium citrate (pH adjusted to 6.95 with orthophosphoric acid), acetonitrile, and methanol as mobile phase, at a flow rate of 1.0 mL min–1, and detection at 228 nm. Separation was complete in less than 10 min. The method was validated for linearity, accuracy, precision, limit of quantitation, and robustness [1, 2]. Linearity, accuracy, and precision were found to be acceptable over the ranges 2.50–30.00 g mL–1 for pioglitazone and 0.10–10.00 g mL–1 for glimepiride. 相似文献
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建立了同时测定牙膏中丹皮酚(Pae)、麝香草酚(Thy)、和厚朴酚(Hon)、厚朴酚(Mag)、甘草次酸(Gly)5种植物源活性成分的超高效液相色谱方法。牙膏样品以90%甲醇为溶剂超声提取,离心取上清液过滤后进行分析,采用Waters ACQUITY UPLCHSS C_(18)(2. 1 mm×100 mm,1. 8μm)为分离柱,乙腈-0. 1%甲酸(pH 2. 8)为流动相,梯度洗脱,流速为0. 3 mL/min,二极管阵列检测器(PDA)的检测波长为275、250nm,外标法定量。结果表明,5种植物源活性成分在2~100 mg/L质量浓度范围内呈良好的线性关系,相关系数(r)均大于0. 999;检出限为0. 2~1. 0 mg/kg,定量下限为0. 8~3. 5 mg/kg;在4个加标水平下的平均回收率为90. 5%~99. 4%,相对标准偏差(RSD)为0. 7%~5. 1%。该法分析快速、重复性好、准确性好、灵敏度高,已应用于实际牙膏样品的测定。 相似文献
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As a biological affinity chromatographic method, cell membrane chromatography (CMC) using a silica stationary phase covered with specific cell membrane has been used in screening active components. The innovation of this work is that the bioactive cell membrane and the chromatographic packing are mixed and absorbed for the first time to form the pre-column. The pre-column was placed in front of a C18 column to create dynamic CMC online high-performance liquid chromatography (HPLC) system. The retention behavior and dynamic changes of pharmaceuticals were studied for this system. The results indicate that the retention time of the drug was increased and the symmetry factor reached the analytical level after the addition of the dynamic cell membrane pre-column. Therefore, the dynamic CMC coupled with HPLC system may be a potentially rapid and efficient drug analysis approach for the interaction of drug molecule and receptor on red blood cell membranes. 相似文献
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《Analytical letters》2012,45(14):2159-2171
A simple method was developed for the determination of hydrophilic whitening agents (ascorbyl glucoside, magnesium ascorbyl phosphate, arbutin, hydroquinone, and kojic acid) in bleaching cosmetics by high performance liquid chromatography with electrochemical detection. The samples were prepared using microdialysis and were separated within ten minutes using isocratic elution. Linear calibration was achieved for concentrations between 0.10 and 10.00 micromolar. The limits of detection were from 0.6 to 2.0 nanomolar; the recoveries were between 91.43 and 108.04 percent, and the relative standard deviation was less than 6.88 percent. This method was used to determine whitening compounds in several cosmetics with on-line microdialysis and the zero net flux method. The procedure was fast, simple, selective, and suitable for routine analysis. 相似文献
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将亲水性较强的C16硅胶反相色谱柱应用于血清样品中β-雌二醇、雌三醇、雌酮和17α-乙炔基雌二醇的分离。实验对分离条件进行了优化,得到的最佳色谱条件是:柱温40℃,流速1mL/min,以40%乙腈水溶液作等度洗脱。在此条件下.4种雌激素可在大约26min内实现基线分离,得到的4个色谱峰峰型对称。分离后的4种雌激素用紫外检测器在200nm处进行测定,方法对β-雌二醇、雌三醇、雌酮和17α-乙炔基雌二醇的检出限分别为0.024、0.015、0.012和0.016mg/L;校正曲线的线性范围为2-3个数量级,相关系数为0.998以上。方法应用于血清样品的测定,β-雌二醇、雌三醇、雌酮和17α-乙炔基雌二醇的标准加入回收率分别为96.3%、103.7%、100.1%和95.2%。 相似文献
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A graphene-based solid-phase extraction (SPE) column was prepared for the isolation of tetracyclines from milk followed by determination by high-performance liquid chromatography. Graphene provided better separation for tetracyclines than amine-modified graphene and carboxyl-modified graphene. The optimized graphene-based SPE column showed high absorption capacities (greater than 4,660?ng) and high recoveries (exceeding 92%) for tetracycline, oxytetracycline, chlortetracycline, and doxycycline and was successfully reused at least fifty times. The limits of detection in milk were from 10 to 20?ng/mL, with recoveries between 82.3 and 103.6%. Furthermore, the system showed superior performance than two commercial SPE cartridges with respect to recovery, purification, and reusability. Therefore, this approach is suitable for the determination of tetracyclines in milk. 相似文献
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高效液相色谱法测定油田水中的非离子表面活性剂 总被引:7,自引:1,他引:6
提出了一种用高效液相色谱法测定油田水中聚氧乙烯辛基苯酚醚-10(OP-10)总量的方法,讨论了固定相和流动相体系的选择、操作参数的优化、共存物对测定的干扰。测定了模拟油田水样品。 相似文献
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《Analytical letters》2012,45(10):2051-2059
ABSTRACT Assay procedures based on UV spectrophotometry and high-performance liquid chromatography (HPLC) have been developed for the determination of meloxicam in tablet formulations. The HPLC method used a reversed-phase C18 column with 0.05M Tris acetic acid buffer - tetrabutylammonium reagent–acetonitrile as eluent, and UV detection at 360nm with isoxicam as the internal standard. The UV method was based on measuring an acidic solution of the drug at 341nm. A comparison was established in terms of linearity, sensitivity, precision, and accuracy. Both methods were simple and rapid. HPLC was more precise and more accurate, the UV technique was slightly faster. 相似文献