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991.
动物尿液中盐酸克伦特罗的分子印迹固相萃取-气相色谱-质谱法研究 总被引:10,自引:0,他引:10
采用分子印迹聚合物(MIP)固相萃取小柱提取、净化并富集猪尿液中的盐酸克伦特罗分子,用N,O-双三甲基硅基三氟乙酰胺(BSTFA)衍生化,毛细管气相色谱-质谱联用(选择离子模式,选择离子为277、262、243和86)对衍生物分析。优化了MIP固相萃取柱的淋洗条件,考察了MIP固相萃取柱的净化效果和消除基体干扰能力,建立了对动物尿液中盐酸克伦特罗的定性、定量分析的方法。在优化条件下,本法检出限(LOD)为0.51μg/L,定量限(LOQ)为1.00μg/L;不同盐酸克伦特罗加入量的回收率为71.0%~89.3%;相对标准偏差为3.2%~9.7%。将该方法与农业行业标准方法比较,结果吻合较好。但该方法灵敏度和精密度高,操作更为简单、快捷。 相似文献
992.
采用石英晶体微天平现场技术,研究了胆红素在纳米TiO2表面的吸附动力学行为,并考察了溶液pH、硅烷亲脂性试剂及金属离子修饰的纳米TiO2对胆红素吸附的影响。结果表明,胆红素在纳米TiO2表面的吸附平衡常数K为2·0×106L/mol;由于亲水性纳米TiO2表面的羟基和胆红素分子中的羧基发生作用,胆红素吸附量随溶液pH增大而增大;但经过硅烷试剂亲脂性修饰后,吸附量随pH增大而下降;经过金属离子修饰后,改变了TiO2表面电荷导致吸附量增加,且吸附量随金属离子电荷增加而增加,当金属离子所带电荷相同时,吸附量基本相同。 相似文献
993.
994.
Chin-Ping Yang Yoshiyuki Oishi Masa-Aki Kakimoto Yoshio Imai 《Journal of polymer science. Part A, Polymer chemistry》1989,27(12):3895-3901
Aromatic polyamides (aramids) having pendant t-butyl group were synthesized by the direct polycondensation of 5-t-butylisophthalic acid with various aromatic diamines in N-methyl-2-pyrrolidone (NMP) using triphenyl phosphite and pyridine as condensing agents. The aramids having inherent viscosities of 0.6–2.4 dL/g were obtained in quantitative yields. These polymers were readily soluble in various solvents such as NMP,N,N-dimethylacetamide, dimethyl sulfoxide, and pyridine, and gave transparent, tough and flexible films by casting from the NMP solutions. The aramids had glass transition temperatures between 250 and 330°C, and started to lose weight around 350°C, with 10% weight loss being recorded at about 450°C in air. 相似文献
995.
996.
Shiow-Ching Chen Meei-Yun Shiue M.-H. Yang 《Analytical and bioanalytical chemistry》1997,357(8):1192-1197
A method is proposed which involves sample pretreatment followed by electrothermal atomic absorption spectrometry (ETAAS)
for determination of cadmium in human urine. A microwave digestion system was devised to accommodate double-closed vessels
for simultaneous digestion of batches of up to 24 urine samples in about 20 min. After digestion, matrix substances which
might interfere were removed using silica-immobilized 8-hydroxyquinoline (I-8HOQ) columns. The analyte adsorbed on the column
was then eluted with dilute nitric acid solution and determined by ETAAS using a fast temperature program. Neither ashing
steps in the furnace heating program nor use of matrix modifiers was necessary. The accuracy, precision, limit of detection,
and sample throughput of the method were evaluated. With meticulous control of systematic errors which may be introduced in
the pretreatment procedures, the present method can serve as a reference technique for the analysis of Cd in urine samples.
Received: 29 July 1996/Revised: 30 September 1996/Accepted: 13 October 1996 相似文献
997.
Shiow-Ching Chen Meei-Yun Shiue M.-H. Yang 《Fresenius' Journal of Analytical Chemistry》1997,357(8):1192-1197
A method is proposed which involves sample pretreatment followed by electrothermal atomic absorption spectrometry (ETAAS)
for determination of cadmium in human urine. A microwave digestion system was devised to accommodate double-closed vessels
for simultaneous digestion of batches of up to 24 urine samples in about 20 min. After digestion, matrix substances which
might interfere were removed using silica-immobilized 8-hydroxyquinoline (I-8HOQ) columns. The analyte adsorbed on the column
was then eluted with dilute nitric acid solution and determined by ETAAS using a fast temperature program. Neither ashing
steps in the furnace heating program nor use of matrix modifiers was necessary. The accuracy, precision, limit of detection,
and sample throughput of the method were evaluated. With meticulous control of systematic errors which may be introduced in
the pretreatment procedures, the present method can serve as a reference technique for the analysis of Cd in urine samples.
Received: 29 July 1996/Revised: 30 September 1996/Accepted: 13 October 1996 相似文献
998.
A method has been described for the direct determinations of trace cadmium using derivative atom trapping flame atomic absorption spectrometry with an improved water-cooled stainless steel trapping equipment. The characteristic concentration (gave a derivative absorbance of 0.0044) and detection limit (3sigma) of cadmium were 0.028 and 0.02 ng ml(-1) when collecting for a 1 min, respectively, which were 992 and 145-fold better than those of the conventional flame atomic absorption spectrometry. The detection limit and sensitivity of the proposed method for a 2 min collection time were 1 and 2 orders of magnitude higher than those of conventional flame atomic absorption spectrometry. The present method was applied to the determinations of cadmium in water samples with a recovery range of 91 approximately 111% and a relative standard deviation of 4.7 approximately 5.6%. 相似文献
999.
LBL分子沉积法制备葡萄糖氧化酶电极 总被引:1,自引:0,他引:1
采用以静电力为主的逐层分子交替沉积技术制备葡萄糖氧化酶(GOD)电极.通过带有正电荷的聚二甲基二烯丙基铵盐酸盐(PDDA)和带有负电荷的GOD交替沉积在修饰有3-巯基-1-丙基磺酸钠(MPS)的金电极表面.以甲酸二茂铁为电子媒介体,用循环伏安法检测GOD电极对葡萄糖的响应.结果表明,当GOD电极组装层数小于4时,电流响应随着层数的增加而增大,超过4层时电流响应减小.其中4层GOD修饰电极的线性范围为0.55~6.63 mmol•L-1,当pH为7.0时,响应最大.同时电极的检测重现性能良好,相对标准偏差为2.4%. 相似文献
1000.
Kai Yang Xuan Zhang Enqin Fu Jingui Qin Minoru Kinoshita 《Journal of solid state chemistry》2004,177(11):4300-4304
Two new intercalation compounds were prepared by the reactions of Ni(II) cyclopolyamine complex cations with a preintercalate Mn1−xPS3K2x(H2O)y, respectively, through “ion exchange” process. Their structures were characterized by elemental analysis, X-ray powder diffraction and infrared spectroscopy. The lattice spacing increased 0.567 and 1.093 nm with respect to the pristine MnPS3. Ferrimagnetism of the intercalates was confirmed by SQUID experiment with Tc at 40 and 33 K, respectively. 相似文献