ICP—AES法测定玩具材料中痕量砷,硒,锑

用电感耦合等离子体原子发射光谱法（ＩＣＰ－ＡＥＳ０测定了玩具材料中的痕量砷，硒和锑。方法简便快速，回收率为９７．５％－１０２．７％，相对标准偏差小于３％。     

毛细管气相色谱法同时测定水产品中的多氯联苯和有机氯农药残留量

建立了毛细管气相色谱法同时测定水产品中多氯联苯和有机氯农药的方法，用高氯酸与冰乙酸的混合溶液消化样品，以石油醚提取，浓硫酸净化后，用毛细管气相色谱法测定，方法的回收法为88％－110％，相对标准偏差为8％－19％（n=6)，检出限为0．08－0．60ug/kg，方法简便，快速，结果准确。     

气相色谱法测定环境空气和废气中的2-丁酮和苯

用活性炭吸附环境空气和废气中的2－丁酮和苯，经二硫化碳解吸后用气相色谱法测定。方法的回收率2－丁酮为86．2％－104．6％， 为91．3％－105．7％。相对标准偏差2－丁酮为2．5％－2．8％，苯为2．5％－3．8％，当采样体积为20L，解吸液体积为2.00ml，进样体积为2μl时，2－丁酮和苯的最低检测浓度分别为0.03mg.m^-3和0.01mg.m^-3。     

反相高效液相色谱分离测定铁—芳烃络合物光引发剂及光解动力学研究

本文以反相高效液相色谱法（ＲＰ－ＨＰＬＣ）研究了铁－芳烃络合物光引发剂及光解产物的分离条件和影响因素，推导出光解动力学方程式，方法灵敏度高，引发剂的检测限为１００ｎｇ／Ｌ，测定的标准偏差为０．３１％～０．４６％，相对标准偏差为０．８２％～２．１３％，在此条件下样品杂质不干扰测定。     

用锌—镉测定天然水中硝酸盐的一种新方法

提出了用锌－镉测定天然水中硝酸盐的一种新方法即通过加入ＮＨ３．Ｈ２Ｏ－ＮＨ４Ｃｌ缓冲液，使硝酸盐的还原率由２０％提高到８７％。方法相对标准偏差为２．１％，检出限为０．１０μｍｏｌ／Ｌ，回收率在９５％－１０２％之间；与镉－铜法相比，两种方法的相对偏差小于８．２％。     

高效液相色谱法测定水体系中N—（2,4—二甲苯基）—N‘—甲基甲脒盐酸盐

本文研究了用高效液相色谱法测定水体中单甲脒盐酸盐的分析方法，峰高定量，标准曲线的线性范围为０－１０００ｍｇ／Ｌ，回收率在８７％－９８％之间，直接进样分析检测限为０．３５ｍｇ／Ｌ。此方法已应用于细胞反应中单甲脒盐酸盐的测定。     

固相萃取高效液相色谱法测定蜂王浆啤酒中的1O-羟基-2-癸烯酸

建立了固相萃取高效液相色谱法测定蜂王浆啤酒中10-羟基-2-癸烯酸含量的方法。采用固相萃取技术富集蜂王浆中的10-羟基-2-癸烯酸,以甲醇-水-磷酸(体积比为50：50：0．5)为流动相,ODS柱分离,用紫外检测器于215nm处检测。10-羟基-2-癸烯酸的浓度在0．5-100．0μg/mL范围内与其色谱峰峰面积呈良好线性关系(r=0．9999),回收率为98％-108％,RSD为2.1％。     

ICP—AES测定钯—钡合金中常量钡

本文采用ＩＣＰ－ＡＥＳ法测定钯－钡合金中常量钡。考察了其体及无机酸的存在对钡发射线强度的影响，采用标准曲线法对含量分别为０．５９％和２６．０４％的两个试样进行了测定，结果满意。     

离子色谱荧光检测法测定废水中痕量2-氨基联苯和4-氨基联苯

采用离子色谱荧光检测法测定废水中的2－氨基联苯（2－ADP）和4－氨基联苯（4－ADP），流动相为1．0mL/min的0．06mol/L NaCl,0.08mol/L HCl,40%(V/V)ACN，分离柱为Dinoex OmniPac PCX-500，该法具有良好的重现性和线性关系，2－ADP和4－ADP的回收率分别为98．5％－101．4％和102．2％－104．0％，检测限分别为0．006mg/L和0．10mg/L。     

微生物电极法测定啤酒中乙醇含量

用自制的乙醇微生物电极建立了一种测定啤酒中乙醇含量的新方法。该法具有良好的精密度和准确度，其测定结果与比重瓶法和气相色谱法相一致，回收率为９７．３％－１０４．９％。该电极线性范围为０．３－１２．０ｍｇ／Ｌ，６０天测定６００余次，其灵敏度基本稳定。测试的最适酸度范围为ｐＨ６．４－７．３，温度为３２－３４℃，测定一个样品需５－８ｍｉｎ。     

蜂王浆超氧化物歧化酶分离纯化及部分性质研究

本文采用硫酸铵盐析、SephedexG-150柱层析从蜂王浆中分离出了超氧化物歧化酶（SOD）。经聚丙烯酰胺凝胶电泳显示单一蛋白区带。此酶比活力为1887 .4U/mg，纯化倍数为524.3，回收率为12.47%，最适pH8.3，最适温度为25℃。Mn^2,Cu^2 ,Ba^2 ,Mg^2 对此酶在有激活作用，Zn^2 则具有抑制作用。过氧化氢和乙醇-氯仿实验表明：蜂王浆中的SOD属Cu/Zn-SOD。     

A novel method developed for acetylcholine detection in royal jelly by using capillary electrophoresis coupled with electrogenerated chemiluminescence based on a simple reaction

A novel method for highly sensitive detection of acetylcholine in royal jelly was proposed by using CE coupled with electrogenerated chemiluminescence (ECL). Acetylcholine, which could not react with Tris(2,2′‐bipyridine)ruthenium(II) to strengthen its ECL signals, decomposed into trimethylamine and strengthened the ECL signals sharply when it was heated to its melting point. This reaction needed no additional reagent and it was mild, simple, stable and rapid, without any side reaction. By combining the above process with CE separation technique, trimethylamine in royal jelly was completely separated from interfering substances and was successfully detected within 4 min. The limit of detection for acetylcholine was found to be 6.3×10^?8 g/mL with a signal‐to‐noise ratio of 3:1. Acetylcholine in the royal jelly was detected to be 912±58 μg/g. The recoveries of acetylcholine chloride in the sample were in the ranges of 92–106%. The coefficients of variation for intra‐day and inter‐day reproducibility were equal to or less than 4.9 and 6.8%, respectively.     

HPLC法快速测定峰皇浆及制品中添加的维生素B6

本文研究了快速、简便测定蜂皇浆及制品中添加的低含量维生素Ｂ_６的ＨＰＬＣ法。称取适量样品，用１０％偏磷酸提取、净化，清液供ＨＰＬＣ分析用。ＷＡＴＥＲＳ荧光检测器，激发波长２９０ｎｍ，发射波长３９０ｎｍ，ＶＢ_６含量在０～１２０ｎｇ之间工作曲线相关系数大于０．９９９，样品中ＶＢ_６含量为０．１％～５％时，方法回收率为９２．１７％～９８．４２％，相对标准偏差（ｎ＝６）小于３．７％。     

揭秘一种卡拉胶魔芋胶果冻

介绍一种卡拉胶-魔芋胶果冻的成分及一般生产工艺流程,着重介绍主要成分κ-卡拉胶、魔芋胶的结构以及在果冻中的作用。     

离子色谱法测定奶制品及蜂王浆中的乙酰胆碱

建立了奶制品及蜂王浆中乙酰胆碱的离子交换/电导检测离子色谱分析方法.样品经去离子水超声提取,离子交换/电导检测离子色谱法测定,外标法定量.采用IonPac CS17(250 mm x4.0 mm i.d.)分析柱,流动相为甲基磺酸,梯度洗脱,流速1.0 mL/min,柱温30℃,检测池温度35℃.实验结果表明,氯化乙酰...     

Separation and determination of 10-hydroxy-2-decenoic acid in royal jelly by capillary electrophoresis

Summary The application of capillary electrophoresis (CE) to the separation and determination of the active ingredient, 10-hydroxy-2-decenoic acid, in royal jelly with direct on-column UV detection at 214 nm is described. Using a cathodic injection and anodic detection scheme, 10-hydroxy-2-decenoic acid (10-HDA) was separated and detected in less than 10 min in a fused silica capillary column with a phosphate buffer at pH 7.3 with an applied voltage of 20 KV followed by direct UV detection. The use of cetyltrimethylammonium bromide (CTAB) as electroosmotic flow modifier allows the rapid separation of 10-HDA from other constituents in royal jelly by reversing the direction of electroosmotic flow. The influence of organic solvents in the electrolyte on separation selectivity is also discussed.     

高效液相色谱-串联质谱法同时测定蜂王浆中氯霉素、甲砜霉素和氟甲砜霉素残留

采用高效液相色谱-串联质谱(HPLC-MS/MS)法同时测定了蜂王浆中氯霉素、甲砜霉素和氟甲砜霉素残留。样品加入阴性蜂蜜和水均质后,采用乙酸乙酯提取,蒸发浓缩,C18固相萃取净化。HPLC分离后,串联质谱法以电喷雾负离子多反应监测方式(MRM)进行定性定量分析。通过对固相萃取条件的优化,大大减小了基质的干扰。氯霉素、氟甲砜霉素和甲砜霉素的检出限分别为0.1 ng/g0、.2 ng/g和0.5 ng/g,平均回收率为89.9%~98.4%,相对标准偏差(RSD)均小于8.2%。     

Determination of tryptophan in bee pollen and royal jelly by high‐performance liquid chromatography with fluorescence detection

A method for tryptophan analysis in bee pollen and royal jelly was developed using HPLC with fluorescence detection. To determine the free tryptophan in bee pollen and royal jelly, ultrasonic extraction was performed using water (pH 6.3)–acetonitrile (10:1, v/v) as extraction solvent. While determining the total tryptophan in these bee products, the method involves alkaline hydrolysis of the proteins with 4 mol/L sodium hydroxide at 110°C for 20 h under anaerobic conditions. The operating conditions for the HPLC analysis were: Symmetry C₁₈ column (4.6 × 250 mm, 5 µm), 0.1% trifluoroacetic acid–methanol (75:25, v/v) as the mobile phase at a flow rate of 1.0 mL/min at 30°C. The fluorescence detector was operated at an excitation wavelength of 280 nm and an emission wavelength of 340 nm. A linear response (r² > 0.9998) was obtained in the range 0.0625–5.0 µg/mL. The method was successfully applied to the determination of the free and total tryptophan contents in bee pollens, which were 0.069 ± 0.003 and 2.693 ± 0.476 mg/g, respectively, while only the total tryptophan was detected in royal jelly, with a content of 1.743 ± 0.066 mg/g. Copyright © 2009 John Wiley & Sons, Ltd.     

高效液相色谱-串联质谱对蜂王浆中27种药物残留的同时测定

建立了蜂王浆中氯霉素、磺胺类、磺胺增效剂、氟喹诺酮类、林可胺类、硝基咪唑类、大环内酯类等7大类27种药物残留的高效液相色谱-串联质谱同时测定的分析方法。对提取溶剂、提取pH值、色谱柱、流动相、质谱条件进行了优化。结果表明,氯霉素的线性范围为0.3~10μg/kg,其余26种药物的线性范围为2~100μg/kg;氯霉素的检出限(S/N=3)为0.1μg/kg,其余26种药物的检出限均为1μg/kg;回收率达70%~119%,相对标准偏差为4.3%~14.9%。该方法满足蜂王浆中27种药物残留的同时测定要求,具有样品预处理简单、灵敏度高、分析时间短的优点。     

气相色谱—质谱法测定蜂王浆及其制品中10—羟基—α—癸烯酸

试样(鲜浆、冻干粉、口服液)经稀盐酸溶液调节pH到3.0以下,以乙醚萃取,用气相色谱-质谱法测定,外标法定量。方法简便、快速、准确,回收率97.6％～98.9％,相对标准偏差2.08％～4.39％。