对磺酸基苯亚甲基若丹宁固相萃取光度法测定水中的汞

研究了对磺酸基苯基亚甲基若丹宁(SBDR)与汞的显色反应,在pH4.0的HAc NaAc缓冲介质中,吐温 80存在下,SBDR与汞反应生成2∶1稳定络合物,该络合物可被WatersPorapak Sep Park C18固相萃取小柱萃取,用乙醇洗脱后在乙醇介质中λmax=520nm,可用分光光度法测定,体系ε=1.16×105L/mol·cm。汞含量在0μg/mL～1.5μg/mL内符合比尔定律,方法可用于水样中汞含量的测定。     

对磺酸基苯亚甲基硫代若丹宁固相萃取光度法测定金的研究

用文献[4]合成的新试剂对磺酸基苯亚甲基硫代若丹宁(SBDTR),研究了SBDTR与金的显色反应。在HCl介质中,乳化剂-OP存在下,SBDTR与金反应生成2∶1稳定络合物,络合物的λmax=540 nm,ε=1.05×105L.mol-1.cm-1,金量在0.1~20μg/10 mL内符合比尔定律,样中的金用TBP萃淋树脂固相萃取柱分离和富集后用该方法测定,方法相对标准偏差为2.2%~3.6%,标准回收率为96%~105%。     

用对磺基苯亚甲基硫代若丹宁为显色剂固相萃取光度法测定环境样品中痕量汞

合成了新试剂对磺基苯亚甲基硫代若丹宁(SBDTR),并用红外光谱、核磁共振氢谱和元素分析鉴定其结构.试验表明:在 pH 3.5 的 HOAc-NaOAc 缓冲介质中,吐温-80 存在下,SBDTR与汞反应生成 2:1 稳定络合物,该络合物可被 Waters Sep-Pak C,18 固相萃取小柱固相萃取,用乙醇洗脱后在乙醇介质中,在此络合物的吸收峰 550 nm 波长处测定其吸光度.体系的摩尔吸光率为 8.42×104L·mol-1·cm-1.汞的质量浓度在 0.1～4.0 mg·L-1 范围内符合比耳定律,应用于河水及食品试样中汞的测定,所得结果与原子吸收光谱法的测定结果相符.     

新试剂SBDR固相萃取光度法测定烟草中汞

在pH为3.5的HOAc-NaOAc缓冲介质中,吐温-80存在下,对磺酸基苯基亚甲基若丹宁(SBDR)与汞反应生成2∶1稳定络合物,该络合物可被Waters Sep-Pak-C18固相萃取小柱萃取,小柱上富集的络合物用1.0 mL无水乙醇洗脱后在乙醇介质中,于其吸收峰550 nm处用1 cm微量比色皿测定吸光度。该显色体系的表观摩尔吸光系数ε=1.05×105L.mol-1.cm-1。汞含量在0~4μg/50 mL内符合比耳定律,方法用于烟草中汞含量的测定,测得RSD(n=7)小于2.5%,回收率在97%~103%之间,测得结果与AAS法测得结果一致。     

对磺酸基苯亚甲基若丹宁光度法测定铝合金中铜

研究了对磺酸基苯亚甲基若丹宁(SBZRN)与铜的显色反应,在pH为5.0的HOAc NaOAc缓冲介质中,SBZRN与铜反应生成2∶1稳定络合物,λmax=510nm,ε=7.48×104L·mol-1·cm-1。铜含量在0～10μg/25ml内符合比耳定律,方法用于铝合金中铜含量的测定,结果满意。     

对磺酸基苯基亚甲基若丹宁光度法测定三乙酸甘油酯中的汞

合成了一种新的若丹宁类试剂对磺酸基苯基亚甲基若丹宁 (SBDR) ,并用红外光谱和元素分析进行结构鉴定。研究了该试剂与汞的显色反应 ,在 p H4.0的HAc- Na Ac缓冲介质中 ,吐温 - 80存在下 ,SBDR与汞反应生成 2∶ 1稳定络合物 ,λmax=5 1 0 nm,ε=1 .0 7× 1 0 5L· mol- 1· cm- 1。汞含量在 0～ 3 0μg/2 5 m L内符合比耳定律。方法用于三乙酸甘油酯中汞含量的测定 ,结果满意。     

对氨基苯亚甲基硫代若丹宁固相萃取分离光度法测定环境水和食品样品中的铅

合成了新试剂对氨基苯亚甲基硫代若丹宁(ABTR),并用红外光谱、核磁共振氢谱和元素分析鉴定其结构。研究了ABTR与铅的显色反应,在pH3.8的HAc NaAc缓冲介质中,吐温80存在下,ABTR与铅反应生成2∶1稳定络合物,该络合物可被WatersSep PakC18小柱固相萃取,小柱上富集的络合物用乙醇洗脱后富集倍数可达50倍,在乙醇介质中,λmax=545nm,体系摩尔吸光系数ε=1.09×105L·mol-1·cm-1。铅量在0.05～4.0μg/mL内符合比尔定律,本法可用于环境水和食品样品中铅的测定。     

固相萃取光度法测定食品中的微量汞

研究了氯磺酚偶氮硫代若丹宁(HSCT)与汞的显色反应,在pH 3.6的HAc-NaAc缓冲介质中,Triton X-100存在下,HSCT与汞反应生成21稳定络合物,该络合物可被C18固相萃取小柱定量萃取,小柱上保留的络合物用四氢呋喃洗脱后用分光光度法测定,λmax=550 nm,体系ε=9.64×104 L/mol/cm.汞含量在0～1.0μg/mL内符合比尔定律,方法可用于食品中痕量汞含量的测定.     

新显色剂邻磺酸基苯偶氮若丹宁合成及与钯的光度法研究

报道了新显色剂邻磺酸基苯偶氮若丹宁（o-SBAR）的合成及其与钯显色反应的性能。在2.4mol· L~(-1)磷酸介质中,试剂与钯形成 1: 1的桔红色配合物,在 520nm波长处配合物有最大吸收,表观摩尔吸光系数为6.65×10~4,反应速度快,选择性高,应用于钯碳催化剂中钯的测定,结果满意。     

Solid Phase Extraction and Spectrophotometric Determination of Mercury in Tobacco and Tobacco Additives with p-Sulfobenzylidenerhodanine as Chromogenic Reagent

A highly sensitive, selective and rapid method for the determination of mercury based on the reaction of mercury(II) with p-sulfobenzylidenerhodanine (SBDR) and the solid phase extraction of the colored chelate with a C₁₈ cartridge has been developed. In the presence of pH 3.8 acetate buffer solution and Tween-80 medium, SBDR reacts with mercury to form a red chelate of a molar ratio of 1:2 (mercury to SBDR). This chelate was enriched by solid phase extraction with a C₁₈ cartridge and eluted from the cartridge with ethanol (containing 5% acetic acid). The enrichment factor of 50 was achieved. In the ethanol medium, the molar absorptivity of the chelate is 1.28×10⁵L·mol^–1·cm^–1 at 545nm. Beers law is obeyed in the range of 0.011.2µgmL^–1 in the measured solution. The relative standard deviation for eleven replicate samples of 0.01µgmL^–1 level is 1.52%. This method can be applied to the determination of mercury in tobacco and tobacco additives with good results.     

微波消解和固相萃取光度法测定氰化渣中痕量钯

根据 2_(2_喹啉偶氮 )_5_二甲氨基苯甲酸 (QADMAB)与钯的显色反应及C18固相萃取小柱对显色络合物的固相萃取 ,并结合微波消解样品 ,建立了一种测定氰化渣中痕量钯的方法。即在pH为 3 5的HAc_NaAc缓冲介质中 ,溴化十六烷基三甲胺 (CTMAB)存在下 ,QADMAB与钯反应生成 2 1稳定络合物 ,该络合物可被C18小柱萃取富集 ,富集的络合物用乙醇洗脱后用光度法测定 ,在乙醇介质中体系λmax=63 0nm ,ε=1 2 0× 1 0 5L·mol-1·cm-1。钯含量在 0 0 1～ 1 5mg L内符合比尔定律 ,方法用于氰化渣中钯含量的测定 ,结果令人满意。     

8-羟基喹哪啶固相萃取光度法测定水样中的铁

研究了8-羟基喹哪啶与铁的显色反应，在pH为8．0的氯化氨-氨水缓冲介质中，在十六烷基三甲基溴化铵(CTMAB)存在下，8-羟基喹哪啶与铁反应生成3：1稳定的蓝紫色络合物，该络合物可被Waters Sep-Park-C18固相萃取小柱萃取，用乙醇洗脱后用光度法测定，络合物λmax=600nm。在此波长下其它金属离子的络合物无光吸收，对铁选择性很好，铁含量在0-5mg/L内符合比尔定律，方法用于水样中痕量铁的测定，结果令人满意。     

Study on the Solid Phase Extraction of Hg(II)‐ABR Chelate with C18 Disks and its Application to the Determination of Mercury in Tobacco and Tobacco Additives

A highly sensitive, selective and rapid method for the determination of mercury based on the rapid reaction of mercury(II) with 5‐(p‐aminobenzylidene)‐rhodanine (ABR) and the solid phase extraction of the colored chelate with C₁₈ disks has been developed. In the presence of pH = 3.5 sodium acetate‐acetic acid buffer solution and Emulsifier‐OP medium, ABR reacts with mercury(II) to form a red chelate of a molar ratio 1:2 (mercury to ABR). This chelate was enriched by the solid phase extraction with C₁₈ disks and eluted the retained chelate from the disks with dimethyl formamide (DMF). The enrichment factor of 50 was achieved. In the DMF medium, the molar absorptivity of the chelate is 1.16 × 10⁵ L.mol^?1.cm^?1 at 540 nm. Beer's law is obeyed in the range of 0.01?3 μg/mL in the measured solution. The relative standard deviation for eleven replicated samples of 0.01 μg/mL level is 1.83%. This method was applied to the determination of mercury in tobacco and tobacco additives with good results.     

2-(2-喹啉偶氮)-1,5-苯二酚固相萃取光度法测定饮用水中铜的研究

根据新试剂2－（2－喹啉偶氮）－1，5－苯二酚（QADHB）与铜的显色反应及Waters Porapak Sep-Park固相萃取小柱对显色络合物的固相萃取，建立了一种测定水样中铜的新方法。在pH=4.0 HAc-NaAc缓冲介质中，溴化十六烷基三甲基铵（CTMAB）存在下，QADHB与铜反应生成2：1稳定络合物，该络合物可用Waters Porapak Sep-Park固相萃取小柱富集，用乙醇洗脱后用光度法测定，可测定水柱中μg/L级的铜。方法用于几种饮用水中铜的分析，结果令人满意。     

固相萃取富集高效液相色谱法测定烟草及烟草添加剂中的重金属元素

报道用固相萃取富集,高效液相色谱法测定烟草及烟草添加剂中镍、铜、锡、铅、镉、汞的方法。样品用微波消化,消化液中的镍、铜、锡、铅、镉、汞用四-(对甲氧基苯基)-卟啉(T4MPP)柱前衍生．用C18固相萃取小柱萃取富集镍、铜、锡、铅、镉、汞的T4MPP络合物,然后用甲醇和四氢呋喃为流动相梯度洗脱,Waters Xterra^TMRP18色谱柱分离二极管阵列检测器检测。镍、铜、锡、铅、隔、汞的捡出限在2～4ng／L之间,方法相对标准偏差为1．8％～2．4％,加标回收率为96％～103％。     

固相萃取—紫外导数光谱法测定血中茚满二酮类抗凝血杀鼠剂

报道了血中敌鼠、氯敌鼠、杀鼠酮的题示测定方法。该法操作简便快速、回收率高，灵敏度较高，萃取使用国产高分子多孔微球ＧＤＸ３０１，价廉易得。三种杀鼠剂以１０ｍｇ／Ｌ量分别加于血中，回收率依次为１００．５％±２．９％、１０１．５％±１．３％及９９．３％±１．５％；血中三种杀鼠剂检出限分别为０．４、０．６及０．４ｍｇ／Ｌ。     

固相萃取-超高效液相色谱法测定水体中4种硝基呋喃类药物

采用固相萃取-超高效液相色谱法测定水体中呋喃西林、呋喃它酮、呋喃妥因、呋喃唑酮等4种硝基呋喃类药物的含量。样品经HLB固相萃取柱净化后,用氨水-甲醇(5+95)溶液洗脱。以BEH C18色谱柱为分离柱,以乙腈和含有0.1%(体积分数)甲酸的2mmol·L-1乙酸铵溶液以体积比23比77组成的混合液为流动相,在检测波长360nm处进行测定。4种硝基呋喃类药物的质量浓度均在5.0~200μg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)为0.02μg·L-1。以空白样品为基体进行加标回收试验,所得回收率在84.5%~97.2%之间,测定值的相对标准偏差(n=6)在1.5%~4.5%之间。     

On-Line Solid Phase Extraction and Spectrophotometric Detection with Flow Technique for the Determination of Nanomolar Level Ammonium in Seawater Samples

The determination of low-level ammonium in seawaters suffers from low sensitivity and high contamination; therefore, it is desirable to develop highly sensitive methods for automatic measurements. A highly sensitive and automated flow technique system for nanomolar level ammonium measurement is described. Reagents for Berthelot reaction were automatically added into seawater samples. After a 10 min reaction at 40°C, the formed indophenol blue compound was on-line extracted onto an Hydrophilic-Lipophilic Balance (HLB) cartridge. The enriched compound was rinsed with water and ethanol solution (30%, v/v) and, in turn, eluted with an eluent containing 30% (v/v) ethanol and 5.0 mM of NaOH, and determined with a spectrophotometer at 640 nm. Parameter, including extraction conditions, reagent concentrations, pH, temperature, and reaction time, were optimized. Under the optimized conditions, the detection limit was 3.5 nM and the linear range was 0–428 nM. The relative standard deviations were 5.7% (n = 8) for 44.6 nM standard solution and less than 6.0% (n = 3–5) for samples within concentrations of about 52.4–288.7 nM; the recovery was in the range 93.6 to 108.5%. The sample throughput was 3 h^?1. The proposed method provides a simple, cheap, and automatic way to determine ammonium in seawater samples without complicated sample treatment.     

Solid Phase Extraction Chemiluminescence Determination of Methamidaphos on Vegetables

IntroductionDuring recent years,organophosphorus pesticides(OPPs)have been widely used in agriculture becauseof their low environmental persistence and high effec-tiveness.However,they have a high acute toxicity.Trace amounts of OPPs may remain in foodstu…