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目的建立检测黏胶剂中苯系物的方法。方法用顶空直接进样气相色谱法测定黏胶剂中的苯、甲苯、乙苯、对二甲苯、间二甲苯、邻二甲苯以及苯乙烯7种组分,对气相色谱柱、顶空加热温度以及顶空提取时间进行了讨论。结果对苯乙烯等7种被测组分的检测限均小于5mg/kg,7种组分在毛细管柱中能够很好的分离,回收率范围为81%~94%,RSD为5%~10%,具有操作简单、快速等特点。结论能够满足对黏胶剂中苯系物测定的分析要求。 相似文献
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建立高效液相色谱-蒸发光散射法(HPLC-ELSD)同时快速测定牛黄中7种组分的含量的方法。色谱柱为UltimateAQ-C18柱,流动相为乙腈-0.2%甲酸水溶液,梯度洗脱,流速1mL/min;蒸发光散射检测器参数:漂移管温度100℃,载气(N2)流速1.9L/min。在选定色谱条件下,胆固醇、各种胆汁酸及其钠盐峰形良好且能达到很好地分离。各组分色谱峰峰面积的对数与浓度的对数呈良好线形关系(r0.9972);标准加入回收率为98.8%~112.7%;7种组分的最低检出限为0.001~0.007g/L。本方法可简便、快速地同时检测不同牛黄样品中7种组分的含量并可表征不同牛黄样品的质量,从而为该名贵药材的质量控制提供更全面的依据和参考。 相似文献
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采用胶束毛细管电动色谱法分离和测定祖师麻中紫丁香苷(SR)、7-甲氧基香豆素(7-MC)、瑞香苷(DN)、瑞香素(DP)和7-羟基香豆素(7-HC)等5种组分,通过研究影响分离和测定的主要因素,建立一种快捷、简便的方法用于5种组分的分离测定.在最佳电泳介质(10 mmol/L SDS pH=9.0,20 mmol/L硼酸盐缓冲溶液)中,5种待测组分在8 min内实现基线分离.SR、7-MC、DN、DP和7-HC的线性响应范围分别为1.0~100、1.5~100、5.0~75、5.0~75和1.0~75!g/mL;检测限分别为0.3、0.5、1.7、1.7和0.3!g/mL.方法成功应用于实际样品祖师麻注射液及祖师麻片中SR、7-MC、DN、DP和7-HC的含量测定. 相似文献
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快速气相色谱法测定食品中的常见防腐剂 总被引:13,自引:0,他引:13
摘要:建立了一种分离测定食品中6种常见防腐剂(山梨酸,苯甲酸,对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯)的简单、准确的快速气相色谱方法,采用长10m,内径100μm的HP-5熔融石英毛细管柱,在快速程序升温条件下,6种常见防腐剂的分析时间为1.3min。各组分平均回收率(n=3)为96.45%;检出限为1.2~10μg/mL;线性相关系数大于0.994。该方法已用于实际食品中防腐剂的检测。 相似文献
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报道了一种芯片毛细管电泳-非接触电导法,用于快速测定葡萄糖氯化钠注射液中两种药物的含量。实验考察了运行缓冲液pH值和分离电压对组分分离的影响,以及检测器激励频率对组分信号响应和灵敏度的影响。确定以20 mmol/L硼酸缓冲液(pH 9.6)为分离介质,分离电压为1 200 V;最佳激励频率为70kHz。在上述条件下,两种成分(葡萄糖和Na+)可在60 s内实现有效分离。Na+和葡萄糖的线性响应范围分别为20~1 000μmol/L和50~5 000μmol/L(r≥0.992);按信噪比(S/N)为3∶1计算检出限分别为8.2μmol/L和26.7μmol/L。两个组分的回收率分别为95%~99%和97%~104%,相对标准偏差(RSDs)均小于4.0%。该文首次报道了葡萄糖和氯化钠两种常见药物成分的同时测定。方法简便、快速、准确度高、稳定性好,用于注射剂含量的测定,结果满意。 相似文献
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混合线性分析法同时测定安痛定注射液中三组分含量 总被引:1,自引:0,他引:1
将一种新近发展的多元校正方法——混合线性分析法,用于安痛定注射液中氨基比林、安替比林、巴比妥含量的同时测定。在220~250nm内取16个波长测量7组标准混合溶液的吸光度矢量作为校正集,以最小二乘法求得系数矢量作为各组分的纯光谱,用混合线性分析法进行数据处理。氨基比林、安替比林、巴比妥的标准回收率分别为99.0%~100.3%、99.0%~100.8%和98.5%~101.1%。用于安痛定注射液中氨基比林、安替比林、巴比妥三组分含量的测定,经t检验,其测定结果与标准法相比,两者间无显著性差异。 相似文献
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M. A. Rodríguez Delgado R. Corbella Tena F. J. García Montelongo 《Chromatographia》1999,50(3-4):235-238
Summary An HPLC method with UV and programmed fluorescence detection has been optimized and used to evaluate the levels of contamination
of PAHs in lightly contaminated biota samples. A specific stationary phase was used that offers high selectivity for PAH separation.
The proposed method was applied to limpet samples from Fuerteventura (Canary Island) with good results. 相似文献
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Solid‐phase extraction combined with dispersive liquid–liquid microextraction for the determination of pyrethroid pesticides in wheat and maize samples
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Xiaodan Zhu Chunhong Jia Zuntao Zheng Xiaoyuan Feng Yue He Ercheng Zhao 《Journal of separation science》2016,39(23):4621-4628
A rapid, selective and sensitive sample preparation method based on solid‐phase extraction combined with the dispersive liquid–liquid microextration was developed for the determination of pyrethroid pesticides in wheat and maize samples. Initially, the samples were extracted with acetonitrile and water solution followed phase separation with the salt addition. The following sample preparation involves a solid‐phase extraction and dispersive liquid–liquid microextraction step, which effectively provide cleanup and enrichment effects. The main experimental factors affecting the performance both of solid‐phase extraction and dispersive liquid–liquid microextration were investigated. The validation results indicated the suitability of the proposed method for routine analyze of pyrethroid pesticides in wheat and maize samples. The fortified recoveries at three levels ranged between 76.4 and 109.8% with relative standard deviations of less than 10.7%. The limit of quantification of the proposed method was below 0.0125 mg/kg for the pyrethoroid pesticides. The proposed method was successfully used for the rapid determination of pyrethroid residues in real wheat and maize samples from crop field in Beijing, China. 相似文献
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反相高效液相色谱法测定可乐、茶叶中的咖啡因 总被引:4,自引:0,他引:4
研究了反相高效液相色谱法(RP-HPLC)直接测定茶叶水提取物、可乐饮料中的咖啡因的新方法,采用PE-C18柱,以CH3OH-H2O-HAc(30:69.92:0.08)溶液作流动相,紫外检测波长为260nm。可在8min内将咖啡因与基体分离,咖啡因含量与峰面积在10μg/mL-100μg/mL范围呈线性关系,回归方程为:Y=33567c(μg/mL)-126421,r=0.9997.该法可用于可乐饮料,茶叶产品质量的监控及产品真伪的辨别。 相似文献
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A thermodynamic consistency test for the vapour-liquid equilibrium data obtained under isobaric conditions is proposed. According
to this procedure, the coexistence equation with correction term for the nonideality of the vapour phase was used. The differential
equation has two singulier points and was solved by numerical integration according to the method predictor-corrector Adams
combined with the classical Runge-Kutta method. The nonideality of the vapour phase is considered by using the second coefficients
from the virial equation of state. The residuals of the vapour phase obtained as differences between the calculated, respectively
experimental values were statistically analysed to detect systematic and random errors. In this order Student and Abbe tests
were used. A study of the influence of the method and the step of the integration is also presented. In this order Runge-Kutta
and Adams methods were compared and for the estimation of the second virial coefficients different published procedures have
been taken into account. In this paper the method of Tsonopoulos and Hayden - O'Connell are taken into account. A correlation
analysis is performed to evaluate the results of this study.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
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《Analytical letters》2012,45(15):2456-2464
A reversed phase high performance liquid chromatographic (RP-HPLC) method with ultraviolet (UV) detector was developed for simultaneously determining five bioactive components (i.e., hydroxysafflor yellow A: HSYA; paeoniflorin, ferulic acid, benzoic acid, and danshensu) in “Xuebijing” (XBJ) injection, a widely used traditional Chinese medicine (TCM) for treating sepsis and multiple organ dysfunction syndrome. A Zorbox SB C18 column was used with 0.2% phosphoric acid (V/V)-acetonitrile as the mobile phase under the condition of gradient elution. The five components were analyzed by using a timed wavelength measure according to their maximum absorption wavelength. The intraday and interday precisions of the five investigated compounds were less than 1.17% and the average recoveries ranged from 97.3% to 103.2%. There were good linear correlations between the concentrations of the five components and their chromatographic peak areas (R2 ≥ 0.9998), the proposed method was successfully applied to determine the five components in different batches of XBJ injection products, the results indicated that the proposed method is simple, stable, and accurate and could be readily utilized as a quality control method for manufacturing process of XBJ injection. 相似文献