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91.
Summary A method is reported for the determination of dibutyltin (DBT), diphenyltin (DPhT), tributyltin (TBT), and triphenyltin (TPhT)
species at the nanogram per litre concentration level in natural water samples. Analytes were isolated from samples by solid-phase
extraction and analysed both off-line and on-line by reversed-phase high-performance liquid chromatography with post-column
derivatization and fluorimetric detection. Several SPE cartridges and eluents were evaluated; C18 enrichment and elution with a mixture of methanol, acetic acid, and water was found most suitable. Preconcentration factors
up to 250 can be achieved when a 500-mL sample is processed. Detection limits, recovery rates, and the precision of the whole
process have been determined. The method has been applied to the determination of organotin species in spiked natural water
samples collected on the NW Mediterranean coast. Recovery rates range from 75 to 110% and detection limits are at the low
ng L−1 level (1–3 ng Sn L−1 for DPhT, DBT, and PhT and 40 ng Sn L−1 for TBT when 250 mL spiked sea water is processed.) 相似文献
92.
93.
建立了测定尿液中3种羟基多环芳烃的氮化碳复合材料磁性固相萃取结合高效液相色谱-荧光检测法。所构筑的磁性氮化碳材料,经扫描电子显微镜、X射线衍射仪、振动样品磁强计和比表面积分析仪表征后,用于尿液中3种羟基多环芳烃的富集净化。考察了吸附剂用量、吸附时间、洗脱溶液和洗脱体积(单次洗脱体积×洗脱次数)对萃取效率的影响。结合高效液相色谱-荧光分析,在0.25~250 μg/L范围内线性关系良好(相关系数r=0.999),3种羟基多环芳烃的检出限和定量限分别为0.08和0.25 μg/L,回收率为90.1%~102%,日内和日间精密度分别为1.5%~7.7%和2.2%~8.7%。该本方法简单、快速、高效,可用于尿液中羟基多环芳烃的分析。 相似文献
94.
建立了一种同时检测塑料食品接触材料中13种紫外吸收剂的超高效合相色谱法。以甲醇为溶剂对塑料食品接触材料样品进行超声提取,经C18固相萃取柱净化,过0.22 μm有机滤膜,采用超高效合相色谱仪分析。选择ACQUTY UPC2 HSS C18 SB色谱柱(150 mm×3.0 mm,1.8 μm),以超临界二氧化碳为流动相,异丙醇为改性剂进行梯度洗脱,在最优色谱条件下,13种紫外吸收剂能够在4 min内实现有效分离。结果表明,在各自线性范围内,13种紫外吸收剂的线性关系良好,标准曲线相关系数不低于0.9985,检出限(S/N=3)为0.05~0.15 mg/kg,加标回收率为86.8%~115.7%,相对标准偏差为0.73%~5.61%。该方法快速简便,准确可靠,同时大大减少了有机溶剂的消耗,可用于塑料食品接触材料中13种紫外吸收剂的快速检测。 相似文献
95.
Meng Wang Weiyue Feng Junwen Shi Fang Zhang Bing Wang Motao Zhu BaiLi Yuliang Zhao Zhifang Chai 《Talanta》2007,71(5):2034-2039
A mild, efficient and convenient extraction method of using 2-mercaptoethanol contained extractant solution combined with an incubator shaker for determination of mercury species in biological samples by HPLC–ICP-MS has been developed. The effects of the concentration of 2-mercaptoethanol, the composition of the extractant solution and the shaking time on the efficiency of mercury extraction were evaluated. The optimization experiments indicated that the quantitative extraction of mercury species from biological samples could be achieved by using 0.1% (v/v) HCl, 0.1% (v/v) 2-mercapoethanol and 0.15% (m/v) KCl extractant solution in an incubator shaker for shaking overnight (about 12 h) at room temperature. The established method was validated by analysis of various biological certified reference materials, including NRCC DOLT-3 (dogfish liver), IAEA 436 (tuna fish), IAEA MA-B-3/TM (garfish filet), IAEA MA-M-2/TM (mussel tissue), GBW 08193 (bovine liver) and GBW 08572 (prawn). The analytical results of the reference materials were in good agreement with the certified or reference values of both methyl and total mercury, indicating that no distinguishable transformation between mercury species had occurred during the extraction and determination procedures. The limit of detection (LOD) for methyl (CH3Hg+) and inorganic mercury (Hg2+) by the method are both as 0.2 μg L−1. The relative standard deviation (R.S.D.s) for CH3Hg+ and Hg2+ are 3.0% and 5.8%, respectively. The advantages of the developed extraction method are that (1) it is easy to operate in HPLC–ICP-MS for mercury species determination since the extracted solution can be directly injected into the HPLC column without pH adjustment and (2) the memory effect of mercury in the ICP-MS measurement system can be reduced. 相似文献
96.
A. E. Goncharov A. A. Politov N. A. Pankrushina O. I. Lomovskii 《Chemistry of Natural Compounds》2006,42(3):336-339
Extracts of Aconitum septentrionale Koelle roots obtained using chloroform, isopropanol, and ethanol were purified using chloroform and basic γ-Al2O3. Ballast materials were selectively adsorbed by γ-Al2O3, increasing the mass fraction of lappaconitine in the extract. The ethanol extract was purified most. The degree of lappaconitine
extraction by chloroform was unaffected by the presence of γ-Al2O3. However, the mass fraction in the extract and lappaconitine extraction from Aconitum septentrionale were increased more than twice.
__________
Translated from Khimiya Prirodnykh Soedinenii, No. 3, pp. 274–276, May–June, 2006. 相似文献
97.
Hiroshi Iwase 《Analytica chimica acta》2002,463(1):21-29
Determination of small amounts of the fat-soluble species Vitamin A (VA) (2.5 μg/g) and β-carotene (9 μg/g) from emulsified nutritional supplements containing 50 kinds of co-existing compounds and a fat content between 2000 and 8000 times higher was performed by solid-phase extraction (SPE) and high-performance liquid chromatography (HPLC) with fluorescence detection set at ex. 350 nm and em. 480 nm, and visible detection at 450 nm using an Inertsil ODS 80A (5 μm) analytical column. Mobile phases of methanol-ethanol (50:50) and acetonitrile-ethanol (70:30) were used for the both vitamins. A Bond Elut C18 cartridge was chosen for SPE after comparison with eight other types of SPE cartridge. Retention time of VA and β-carotene was 7 and 8 min, respectively, giving a limit of detection of ca. 0.1 ng per injection at a signal-to-noise ratio 3:1. Recoveries of VA and β-carotene were over 90% by the standard addition method. Relative standard deviation of VA and β-carotene were ca. 2.9 (n=5) and 2.3% (n=5), respectively. 相似文献
98.
99.
100.
毛细管电泳法研究提取剂对黄连-黄柏共煎剂中生物碱含量的影响 总被引:4,自引:0,他引:4
用毛细管电泳法,对黄连与黄柏配伍后共煎剂中的主要生物碱进行了分析。以50 mmol/L Na2B4O7(pH=7)-CH3OH(85:15,V/V)为背景电解质,操作电压为14 kV,电迁移进样10 kV×5s,柱上223 nm检测,5种主要生物碱9 min内可在50 cm×75μm毛细管上实现基线分离。以小檗碱、巴马汀的提取量为指标,分析了提取剂对提取效果的影响。以30%的乙醇水溶液为提取剂,可得到最大煎出量。 相似文献