Turbidimetric Titration of Ethyl Acetate Extracts of Halo- and Aminobenzoic Acids

The extraction of halo- and aminobenzoic acids from aqueous solutions with a hydrophilic solvent (ethyl acetate) was studied. Conditions for turbidimetric titration of these acids in the organic extract were optimized. Procedures for reliable nonaqueous titration of acids were developed.     

Studies on the Determination of Mercury by On-line Solvent Extraction and Non-Aqueous Media Hydride Generation Non-Dispersive Atomic Fluorescence Spectrometry

A new method for on-line solvent extraction covalent hydride generation in a non-aqueous extraction phase is proposed. Both liquid–liquid extraction and gas–liquid separation steps are accomplished in an online mode and with AFS as detector. Hydride generation is carried out in an aliquot of metal-complex extraction solution by sodium tetrahydroborate in N,N-dimethylformamide solution and anhydrous acetic acid. An improved U-type gas–liquid separator was used. The working conditions and manifolds scheme of flow injection were optimized. The detection limit attained for mercury was 20ngL^–1. The precision of the determination at a concentration level of around 20 times the detection limit was 5.6%. The proposed method gives improved sensitivity and eliminates interference. The method has been applied to the determination of mercury in certified reference materials with good accuracy and precision.     

Determination of Chlorophenols in Sediments Using Ultrasonic Solvent Extraction Followed by Stir Bar Sorptive Extraction Coupled to TD-GC-MS

A rapid method for analysis of chlorophenol content in sediments was developed using ultrasonic solvent extraction followed by stir bar sorptive extraction. The sediment sample is extracted using methanol and dichloromethane (9:1) in an ultrasonic bath. The extract is then redissolved in water and phenolic compounds are derivatised using acetic acid anhydride. The derivates are preconcentrated on a stir bar coated with polydimethylsiloxane that is commercially available as Gerstel Twister which is then thermally desorbed and analysed by GC-MS. Method performance is illustrated and evaluated for the enrichment of up to 100 ng g⁻¹ of selected chlorophenols in freshwater sediment samples. The method showed good linearity, recoveries and blank levels, as well as advantages such as sensitivity, simplicity, low cost and high feasibility.

     

ASE-HPLC检测某型号球形发射药中的叠氮硝胺、硝化甘油、Ⅱ号中定剂含量的研究

采用快速溶剂萃取(ASE)技术和高效液相色谱法测定某球形药中叠氮硝胺(DIANP)、硝化甘油(NG)和II号中定剂(C2)的含量.ASE提取条件:二氯甲烷做萃取溶剂,萃取温度100℃,静态萃取10 min,萃取2次.HPLC测定条件:YWG C18柱(150×4.6 mm,10μm),以甲醇和水作为流动相,梯度洗脱,流速1 mL/min,检测波长210nm.测定结果表明DIANP、NG、C2平均回收率分别为99.6%、100.3%、99.4%,RSD分别为0.7%、0.8%、0.9%(n=5),检出限分别为2.1、1.5和0.2 mg/L,线性范围分别为0.02~0.98 g/L,0.03~1.38 g/L,0.002~0.124g/L.用此方法共检测某批球形发射药样品5份,检测结果与滴析-HPLC法检测结果相当.     

非水滴定法测定酰胺缩醛

对非水滴定酰胺缩醛的溶剂、滴定剂和指示剂进行了选择试验，用ＨＣｌ甲醇标准液进行滴定，通过电位滴定曲线或甲基橙指示剂可以准确的确定滴定终点，方法简便，结果准确。     

加速溶剂萃取/HPLC-MS对毛冬青药材中Ilexgenin A与Ilexsaponin A1含量的测定

建立了加速溶剂萃取/高效液相色谱-质谱法(ASE/HPLC-MS)测定毛冬青药材中活性成分ilexgenin A和ilexsaponin A1含量的方法.采用ASE萃取毛冬青药材中的活性成分ilexgenin A和ilexsaponin A1,萃取溶剂为甲醇,萃取温度100 ℃,压力1.0×107 Pa,静态萃取模式,循环3次,每次萃取10 min.采用HPLC-MS对萃取液中ilexgenin A和ilexsaponin A1进行定量分析,色谱柱选用Dikma Diamonsil C18(4.6 mm×250 mm,5 μm),以水和乙腈为流动相进行梯度洗脱,大气压化学电离源(APCI),定量离子m/z 485.ilexgenin A和ilexsaponin A1的线性范围为1.0 ～200.0 mg/L,对毛冬青试样的定量下限分别为19.5和35.0 μg/g,RSD分别为6.7%和7.8%,回收率分别为87% ～96%和93% ～102%.将建立的方法用于分析11个不同产地的毛冬青药材,ilexgenin A含量为0.42 ～6.3 mg/g,ilexsaponin A1含量为0.80 ～8.9 mg/g.     

非水库仑滴定法测定锂电池电解液中游离酸的含量

锂电池因具有能量密度大、电压高和记忆效应小等优点,被广泛用于新能源汽车的制造,其中六氟磷酸锂(LiPF6)电解液是该电池的重要组成部分,其质量属性决定了锂电池的性能差异[1-2]。由于六氟磷酸锂稳定性较差,易发生水解和热分解,导致电解液中的游离酸含量上升,进而影响电池的容量.     

固相萃取-离子色谱-积分脉冲安培法测定人血清中游离氨基酸

比较了磺基水杨酸和无水甲醇沉淀人血清中蛋白质的效果,优化了国产732型阳离子交换树脂进行固相萃取净化的条件和Dionex-600离子色谱分析系统的梯度淋洗条件。用该离子色谱仪检测了谷氨酰胺等14种氨基酸,结果表明,峰面积-浓度的校正曲线的相关系数为0.9900~0.9995,检出限为0.02~0.59mg/L;峰面积的相对标准偏差为1.9%~10.4%;回收率为80.6%~114.8%。     

Phosphatidylcholine-Gramicidin a Interaction Study in Non-Aqueous Solvent with a new HPLC-SEC Column

Abstract

A new HPLC-SEC column, Ultrastyragel 500 Å, has been assayed in order to check the separation between gramicidin A and phosphatidylcholine in tetrahydrofuran. The good resolution of both compounds has allowed the quantitation of lipid-polypeptide interaction in terms of the binding ratio parameter, BR. A BR value of 3.6 moles of phosphatidylcholine per mole of gramicidin A has been obtained for a 0.1 % (w/v) phosphatidylcholine solution as eluent. The suitability of this support for studies on lipid-polypeptide interactions in non-aqueous solvents is demonstrated.     

电位滴定法测定定心藤中总有机酸的含量

为研究定心藤中总有机酸的最佳提取工艺,建立其测定方法,采用正交实验法考察了乙醇含量、固液比、提取时间及提取次数4个因素对该工艺的影响,利用电位滴定法对其进行了测定。结果表明,定心藤中总有机酸提取的最佳提取工艺为:乙醇含量75%,固液比1∶10,提取时间2.5 h,提取次数3次;电位滴定法对其测定简单可行,精密度高,重现性好,为定心藤进一步研究和资源开发利用提供一定的科学依据。     

两点电位滴定法在非水滴定中的应用

硝酸舍他康唑主要用于治疗浅表性真菌新药,加巴喷丁是近20年来开发出能增强神经抑制和构思,控制神经兴奋的新一代抗癫痫药物,目前广泛应用于难治性癫痫等病历[1]。两种药物含量测定方法为高氯酸非水电位滴定。传统电位滴定法需要以较小的滴定体积间隔测定大量的滴定数据,数据处理比较繁琐,给实际应用带来诸多不便。在前人研究基础上,提出了识别电位滴定终点的方法并进行了实际应用[2-4]。依据该法,只需在滴定计量点前附近记录两次标准溶液体积和相应电极电位值,利用公式即可计算化学计量点。经对硝酸舍他康唑与加巴喷丁测定,方法精密度与准…     

水中痕量土霉素的亲水溶剂浮选-分光光度测定

本文利用自制的浮选装置,选择四氢呋喃和无水乙醇(4+1)混合溶液作溶剂,氯化钠作分相剂,将Fe(Ⅲ)与土霉素(OTC)形成的疏水性缔合物浮选至有机相,然后采用分光光度法测定,方法线性线性范围为6.6×10~(-7)～3.4×10~(-5) mol/L;检出限为3.63×10~(-7) mol/L;平均回收率为99.95%;表观摩尔吸光系数ε=2.028×10~5 L·5moL~(-1)·5cm~(-1).该方法设备简单、测定快速、灵敏度高、分离物质易于提取和不产生二次污染,可用于环境水样中痕量土霉素的快速测定.     

溶剂浮选-HPLC法测定茵陈中滨蒿内酯的研究

摘要：建立茵陈中滨蒿内酯的溶剂浮选分离富集方法。方法 考察了浮选溶剂、氮气流速、试液 pH、浮选时间及电解质 NaCl 等因素对浮选效果的影响,优选出最佳浮选条件,并由高效液相色谱测定其含量。结果 对最佳条件下的浮选效果进行了评价。结论 加标回收率92.31 ~ 99.97 %; RSD = 3.20 %.溶剂浮选分离富集方法可行。     

溶剂萃取-气相色谱法测定粮食中硫丹类农药残留量

提出了粮食中α-硫丹、β-硫丹、硫丹乙酯、硫丹丙酯和硫丹硫酸盐5种硫丹类有机氯农药的气相色谱测定方法。样品粉碎后以丙酮为溶剂经快速溶剂萃取仪在加热(80℃)状态下静态提取5min、氟罗里硅土固相萃取柱净化后注入毛细管气相色谱仪分离测定。5种硫丹类农药的测定下限(10S/N)分别为0.82～1.75μg.kg-1,平均回收率为88.9%～99.1%,相对标准偏差(n=5)为6.80%～10.23%。     

溶剂萃取-毛细管气相色谱法测定烟草中主要生物碱

报道了用毛细管柱气相色谱同时测定烟草中尼古丁、去甲基尼古丁、新烟碱和去氢新烟碱4种主要生物碱的方法。烟草样品经二氯甲烷／甲醇(V/V,3：1)溶剂萃取,过一次性滤膜,直接进样,经HP-5MS毛细管柱分离,氮磷检测器(NPD)检测。该方法简单,重现性好;4种生物碱相对标准偏差为1．5％～3．4％;加标回收率为93．6％～102．4％。