正交试验优化-顶空固相微萃取-气相色谱-串联质谱法测定水中戊二醛

建立了顶空固相微萃取-气相色谱-串联质谱测定水中戊二醛的方法。设计5因素4水平完整的正交试验,通过极差分析获得顶空固相微萃取优化条件。10 mL,pH 1的水样加入6 g NaCl,经非极性PDM S,100μm纤维头于75℃萃取25 min,210℃解析进样0.2 min。采用VF-5(60 m×0.25 mm×0.25μm)色谱柱程序升温分离,选择多反应监测(M RM)模式采集质谱信息。以m/z 82/54为定量离子,以m/z 82/39为定性离子,外标法定量。结果表明,戊二醛质量浓度在0.02~0.6 mg/L范围内线性良好,相关系数(r)>0.9996,方法检出限7μg/L,定量限20μg/L。低(0.04 mg/L)、中(0.1 mg/L)、高(0.4 mg/L)3个水平加标回收率为87.4%~103.7%,相对标准偏差(RSD)<6%。方法适用于测定水中的戊二醛。     

GC—TOF／MS及主成分投影法用于安息香膏的成分分析

利用气相色谱-飞行时间质谱,对安息香膏的挥发性成分进行分析,并用峰面积归一化法计算各成分相对含量。利用在两种不同极性色谱柱上的比较试验,确定了适合安息香膏分析的色谱柱条件。在最适合安息香膏分离的色谱条件下对4种不同批次安息香膏的微差样品进行分析。通过质谱库检索,辅助英文版精油库（ES02006版）比对,解析并确定出精油中的24种组分,主要成分是苯甲酸苄酯（25．52％）、苯甲酸（23．12％）、乙基香兰素（14．93％）、苯甲醇（14．50％）、肉桂酸肉桂酯（13．41％）、肉桂酸苄酯（7．54％）等。用主成分投影分析法对4种微差样品进行分类区分,结果证明,用主成分分析法辅助GC—TOF／MS能较快速准确地对微差样品进行区分。该方法可用于安息香膏的产品开发及其品质控书1。     

Synthesis and Characterization of Chloropentaaryloxycyclotriphosphazene Derivatives

Five chloropentaaryloxycyclotriphosphazene derivatives were synthesized by the reaction of hexachlorocyclotriphosphazene with potassium phenoxide in tetrahydrofuran. A satisfactory yield could be obtained when a 5.1 : 1(KOC ₆ H ₄ R : P ₃ N ₃ Cl ₆ ) molar ratio was used. The new compounds were characterized by IR, ¹H NMR, ³¹P NMR, ¹³C NMR, and ESI-MS, and for two of them by HR-MS.     

Highly Regioselective Synthesis of Novel 4-O-Phosphorylated Paeonol Analogs

Abstract

4-O-phosphorylated paeonol derivatives were conveniently prepared by a facile method. Resacetophenone was prepared by the Friedel–Crafts acylation reaction of acetic acid with resorcinol. It was then phosphorylated regioselectively at the 4-O position using the Atherton–Todd reaction. An efficient, highly regioselective method to synthesize 4-O-phosphorylated paeonol derivatives is provided, and the approach has the merits of mild reaction conditions.

Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.     

Radioactive ion beam line in Lanzhou

Radioactive ion beam line in Lanzhou (RIBLL) has been constructed for the production of short-lived radioactive nuclei and studies of exotic nuclei far from the β-stability line. It has been put into operation recently at the National Laboratory of Heavy Ion Accelerator Lanzhou. RIBLL consists of two doubly achromatic parts with a solid acceptance ΔΩ⩾6.5 msr, momentum acceptance Δp/p=±5% and maximum magnetic rigidityBp _max=4.2 Tm. The second part of RIBLL serving as a spectrometer gives an element resolutionZ/ΔZ>150 and mass resolutionA/ΔA>300. The polarized secondary beams can be obtained by using a swinger dipole magnet to change the incident direction of primary projectile from 0° to 5°. The shortest lift time for secondary beams on RIBLL is less than 1 μs. First experiments were performed with neutron rich nuclei for understanding the properties of halo nuclei and exotic nuclear reactions. Project supported by the Chinese Academy of Sciences, the State Science and Technology Commission of China, the National Natural Science Foundation of China (Grant No. 19675055).