蒙成药吉如很阿嘎如-8中多糖的组分和糖含量

本文介绍了提取吉如很阿嘎如－8中水溶性多糖的方法，并用硫酸－苯酚法测定了该药中水溶性多糖的含量。回收率为99．3％－100．5％，RSD为0．90％。用气相色谱法测定了吉如很阿嘎如－8的水溶性多糖，它是由阿拉伯糖、木糖、甘露糖、半乳糖、葡萄糖等组成。它们的摩尔比为：1．00：0．76：3．61：2．88：5．00。     

微量化提取结合毛细管柱气相色谱法测定茶叶中六六六、滴滴涕残留量的探讨

微量化提取结合毛细管柱气相色谱法测定茶叶中六六六，滴滴涕残留量，对六六六，滴滴涕8种异构体都能得到满意的分离效果，采用外标法定量测定，且用此方法检测滴滴涕4种异构体的平均回收率在92．5％－103．2％之间，相对标准偏差在1．6％－3．1％之间，检出限可达0．04μg/kg.     

吸附/热解吸/气相色谱法测定环境空气中的丙烯酸甲酯

用ＴｅｎａｘＧＣ吸附环境空气中的丙烯酸甲酯,热解吸／气相色谱法测定,方法的回收率为８７．４％－１０８．９％,相对标准偏差为４．７％－６．３％,当采样体积２Ｌ时,最低检测质量浓度为０．０１ｍｇ／ｍ＾３。     

气相色谱法测定花生油中微量多氯联苯(PCB)

本文采用液－液萃取技术提取花生油中微量多氯联苯，用毛细管柱气相色谱法进行测定。整个过程只需３２ｍｉｎ，本方法最低检出限为１．００μｇ／ｋｇ     

超声提取-反相高效液相色谱法测定牛膝中蜕皮甾酮

比较了超声提取与回流提取法在提取牛膝中活性成分蜕皮甾酮的提取效率，在频率为1100kHz时超声提取40min可获得稳定的提取效率。采用Shim-Pack CLC-ODS色谱柱，甲醇：水＝40：60（V／V，％）为流动相，在波长248nm下，测定牛膝中蜕皮甾酮，线性范围为2－200μg/mL（r=0．9998），检出限为0．052μg/mL（S/n=3），加标加收率为98．3％－103％。     

流动注射在线沉淀预富集原子吸收间接法测定蜂蛹中黄酮

本文研究了流动注射在线沉淀预富集原子吸收法间接测定生物样品中黄酮的实验条件,流程参数,探讨了不同提取条件下蜂蛹中黄酮类化合物的提取效率及其影响。采用甲醇冷浸－碱液浸取联合提取,提取率９８．８％,将微型沉淀预富集柱用于蜂蛹中黄酮类化合物的测定ＲＳＤ为２．８％,加标回收率为９５．８％￣１０４．０％。     

1,1,1,2,3,3,3─七氟丙烷的气相声速

分析了气相声速与理想气体比定压热容的热力学关系,用超声变程干涉仪测定了１,１,１,２,３,３,３－七氟丙烷（ＨＦＣ－２２７ｅａ）的 ７２组气相声速值,温度范围 ２７３－３３３ Ｋ,压力范围 ２６－３１５ ｋＰａ,测量不确定度小于 ０．０５％。根据这些实验数据,确定了ＨＦＣ－２２７ｅａ的理想气体比定压热容和声速第二维里系数,并分别拟合得到了与温度的函数,理想气体比定压热容的不确定度小于 ０．５％．使用方阱势能模型导出了 ＨＦＣ－２２７ｅａ的第二维里系数,并与文献值进行了比较。     

气相色谱法测定柑橘与土壤中氟啶虫胺腈的残留量

建立了柑橘和土壤中氟啶虫胺腈残留量的气相色谱测定方法.柑橘全果、果肉和土壤样品中的氟啶虫胺腈用乙腈提取,果皮样品用乙腈-水(4:1,V/V)混合溶剂提取,经中性氧化铝柱净化,浓缩后采用气相色谱-电子捕获检测器(GC-ECD)检测,结果表明,在添加浓度为0.05-1.0mg/kg时,氟啶虫胺腈在样品中的平均回收率为81.3％-101.2％,相对标准偏差为0.9％-4.9％.方法的检出限(LOD)为5.0× 10-11g,氟啶虫胺腈在全果、果肉、果皮和土壤中的最低检测浓度(LOQ)为0.05mg/kg.该方法杂质干扰少,准确性及灵敏度满足农药残留检测的基本要求,对检测硬件要求低,适用于柑橘和土壤中氟啶虫胺腈残留的分析.     

原子吸收光谱法测定鸡蛋中营养元素的前处理方法研究

本文分别采用０．１ｍｏｌ·Ｌ－１盐酸、６ｍｏｌ·Ｌ－１盐酸、ｐＨ７．０１ｍｏｌ·Ｌ－１ＮＨ４Ａｃ振荡提取及６ｍｏｌ·Ｌ－１盐酸煮沸法测定了鸡蛋中Ｋ、Ｎａ、Ｍｇ、Ｃａ、Ｚｎ、Ｆｅ、Ｍｎ、Ｃｕ八种元素,并与经典前处理方法即现在普遍采用的浓硝酸－高氯酸全消化法及干灰法进行比较,结果表明,对于大量元素Ｋ、Ｎａ、Ｍｇ几种提取方法与经典法接近,回收率达９０％～１１５％;微量元素Ｚｎ、Ｍｎ、Ｆｅ也可分别用ｐＨ７．０１ｍｏｌ·Ｌ－１ＮＨ４Ａｃ,０．１ｍｏｌ·Ｌ－１盐酸、６ｍｏｌ·Ｌ－１盐酸振荡提取,回收率在１００％～１１５％之间,Ｃｕ则可用６ｍｏｌ·Ｌ－１盐酸煮沸法测定,回收率较理想。而Ｃａ这几种方法提取结果均不理想,主要因增感作用,造成结果偏高。经典干灰化结果偏低,灰化温度达４５０℃,即可造成多种元素损失,且繁琐费时。本文采用的几种提取方法简单、快速,结果准确性、精度可达到分析要求。     

色谱－质谱联用分析大气颗粒中多环芳烃

采用毛细管气相色谱－质谱联用技术（ＧＣ／ＭＳ）．结合溶剂提取和柱色层分离方法，分析了抚顺市采暖期与非采暖期大气颗粒物样品中多环芳烃的化学组成，结果表明，采暧期多环芳烃种类明显多于非采暖期，其中具有致癌活性的物质约１０种，占总组成的２５％。     

液相色谱法同时测定辛硫磷和氯氰菊酯

本文采用高效液相色谱分析，在ODS柱上，用甲醇／水（85／15）洗脱，检测波长为254nm，对辛硫磷和氯氰菊酯复配农药－20％辛氯乳油的分析方法进行了研究，方法的相对标准偏差小于0．36％，线性范围为1．5－300mg/L。该方法简便、快速、准确，是理想的的质控分析方法。     

Determination of Organophosphorus Pesticide Residues in Vegetables by Electrokinetic Sequential Injection Analysis

A fast and convenient analysis method based on a plant esterase reaction inhibited by organophosphorus pesticides was developed for the determination of the pesticide residues in vegetable samples. The proposed method was performed with an electrokinetic sequential injection analysis (ESIA) system, which consisted of a spectrophotometer, a homemade electro‐osmosis pump, and four solenoid valves controlled by a Visual C program. The plant esterase extracted from fresh flour was adopted in the enzyme reaction. Several reaction parameters, such as the sample volume, the length of reaction coil, and the concentrations of reactants, are discussed in detail. The linear range of the calibration concentration was 0.03–0.5 µg/g dimethoate, which was used as a converted concentration of total organophosphorus pesticides. The detection limit of 0.01 µg/g dimethoate was achieved. The analytical throughput of the proposed method was about 24 samples per hour.     

Photochemically-Induced Fluorescence Properties of Two Benzoyl- and Phenylurea Pesticides and Determination in Natural Waters

A photo-induced fluorescence (PIF) method was developed for the determination of two benzoyl- and phenylurea pesticides, namely diflubenzuron (DFB) and fenuron (FEN). The photoconversion under UV irradiation of both pesticides into strongly fluorescent photoproducts was performed in several media (methanol, ethanol, acetonitrile, pH4 aqueous solution and pH4 water–methanol (30:70, v/v) mixture). PIF parameters were optimized. Analytical figures of merit for the PIF determination of DFB and FEN were satisfactory, with rather wide linear dynamic range (LDR) values of one to two orders of magnitude, relatively low limit of detection (LOD) values of, respectively, 9–24 ng/mL for DFB and 1–28 ng/mL for FEN, and limit of quantification (LOQ) values of, respectively, 30–80 ng/mL for DFB and 4–95 ng/mL for FEN, according to the medium. Relative standard deviation (RSD) values were in the range 1.7–5.6 %. PIF was validated by comparing its analytical performances to those of a standard UV absorption spectrophotometric method. The optimized PIF method was applied to the quantitative analysis of both pesticides in various spiked natural water samples collected in a Senegal agricultural area by the standard addition procedure prior to extraction steps in dichloromethane, with satisfactory mean recovery percentage values (97.0–105.3 for DFB and 98.3–102.8 % for FEN). An interference study of foreign species, including pesticides and inorganic ions, likely to be present in natural waters, was also carried out.     

超高效液相色谱串联质谱技术测定麦芽中的赤霉酸

利用超高效液相色谱串联质谱技术检测啤酒原料麦芽中的赤霉酸(Gibberellic acid,GA3)。样品由乙腈/水(80/20)提取后,经Oasis MAX固相萃取柱净化,以甲醇-甲酸水为流动相,梯度洗脱下,经选择离子模式(SIR)检测。结果表明,赤霉酸在ACQUITY UPLCTMBEH C18色谱柱上(2.1mm×100mm,1.7μm)得到较好分离,回收率为70%—78%,检出限0.6μg/L,RSD≤8.9%,该方法适用于麦芽等复杂体系中微量赤霉酸的检测。     

液-液萃取与气相色谱-质谱联用测定环境样品中的单质硫

采用液-液萃取与气相色谱-质谱联用测定复杂环境基质样品中的单质硫,研究萃取溶剂、色谱柱类型及炉温升温程序对分析方法的影响。实验结果表明:二硫化碳作为萃取溶剂好于四氯化碳。采用HP-1MS柱时,炉温在270℃恒温保持10min进行分析,单质硫峰形较好。采用HP-5MS柱,单质硫峰形及丰度均优于HP-1M S柱。该分析方法的线性范围为5—200mg/L,可决系数R2为0.9980,最低定量限0.106mg/L,测定5个5mg/L硫水混合液平行样的相对标准偏差为3.179%。生物脱硫反应器出水中单质硫测定结果表明,该检测方法是可行的。     

RP-HPLC测定不同β-环糊精衍生物超分子包合物中丹皮酚的含量

建立了用反相高效液相色谱法测定羟丙基-β-环糊精（HP-β-CD）、甲基-β-环糊精（M-β-CD）以及取代度为1、4、7的3种磺丙基醚-β-环糊精（SPE1-β-CD、SPE4-β-CD、SPE7-β-CD）与丹皮酚（PAE）所形成的超分子包合物中丹皮酚含量的方法。采用Extend C18色谱柱（4.6mm×150mm,5μm）,流动相为甲醇-水（50∶50）,检测波长274nm,流速1mL/min,柱温为25℃。结果表明丹皮酚在4.98—79.68μg/mL浓度范围内线性关系良好（R^2=0.9999）;平均加标回收率分别为96.78%、95.91%、100.57%、99.71%、100.70%;RSD分别为0.92%、1.76%、0.88%、1.69%、0.96%（n=6）。本法可用于β-环糊精衍生物/丹皮酚超分子包合物中丹皮酚的含量测定。     

甜茶叶中甜茶苷的UPLC-MS/MS分析

采用超高效液相色谱-质谱联用法测定广西特产甜茶叶中的主要甜味成分甜茶苷的含量.样品经前处理后以Acquity UPLC BEH C18柱为色谱柱,流动相为乙腈(含体积分数为0.1％甲酸)-蒸馏水(含体积分数0.1％甲酸),梯度条件为10min乙腈相体积由20％变化到65％,柱温35℃,进样量5μL,流速为0.15mL/...     

Determination of pesticides in honey by ultrasonic solvent extraction and thin-layer chromatography

A rapid method for quantitative determination of atrazine and simazine in honey samples was investigated. The procedure was based on the extraction of pesticides by sonication with benzene:water = 1:1 (v/v) mixture, thin-layer chromatographic separation and quantification by CAMAG Video Documentation system in conjunction with the Reprostar 3. The extraction procedure was optimized with regard to the amount of solvent, duration of sonication and the number of extraction steps. The apparent recovery of pesticides from honey was 92.3 ± 2.4 for atrazine and 94.2 ± 2.8 for simazine, when they were extracted in three steps for 20 min using 20 ml of solvent. Ultrasonic solvent extraction was compared with traditional shake-flask extraction method.     

反相高效液相色谱法测定清开灵分散片中栀子苷含量

对中药复方制剂清开灵分散片中有效成分栀子苷进行含量测定。采用反相高效液相色谱法,Agilent1100ZORBAXEclipseXDB-C18色谱柱(4.6mm×150mm,5μm),乙腈-水(15∶85,V/V)为流动相,检测波长为238nm,流速1.0mL/min,柱温25℃。栀子苷在0.0593—1.4825μg.mL-1范围内与峰面积呈良好的线性关系,r=0.9999,平均加样回收率为98.93%(n=6),RSD=1.21%。该方法快速简便、灵敏度和稳定性高,可有效控制清开灵分散片的内在质量。     

高效液相色谱法测定烟火药剂中的苦味酸

建立了烟火药剂中苦味酸的高效液相色谱检测方法。采用Zorbax Eclipse XDB-C18色谱柱（4.6mm×250mm,5μm）分离,V（甲醇）∶V（0.1%冰醋酸水溶液）=55∶45,等梯度洗脱,流速0.8mL/min;测定温度为40℃;采用紫外检测器检测,检测波长为350nm。苦味酸的质量浓度在0.5—20mg/L时与色谱峰面积之间线性关系良好（r=0.9998）;加标回收率为85.6%—92.4%,相对标准偏差（RSD）为2.1%—6.5%。该方法简便快速,结果准确,重现性好,可作为检测烟火药剂中苦味酸的一个有效方法。