First mass measurement of short-lived nuclides at HIRFL-CSR

Recent commissioning of the HIRFL-CSR has demonstrated its ability to perform direct mass measurement for short-lived nuclides. Projectile fragments produced by the 78Kr ions at 481.88 MeV/u were separated with the new radioactive beam line in Lanzhou （RIBLL2）, and injected into and stored in the experimental storage ring （CSRe）. By operating the CSRe as an isochronous mass spectrometry, a typical mass resolution around 2.0×10？5 has been achieved. The masses for 63Ge, 65As and 67Se were measured for the first time. The measured masses are compared with theoretical predictions and the location of the proton drip-line for As isotopes is discussed. The implication of the 65As mass in the astrophysical rapid proton capture process has also been addressed.     

固相微萃取-气相色谱-质谱联用测定人血清中游离脂肪酸

采用甲基丙烯酸丁酯-羟基硅油(BMA/OH-TSO)固相微萃取探头(SPME)与气相色谱-质谱(GC-MS)联用测定人血清中游离脂肪酸的含量.用H2SO4-甲醇对血清中游离脂肪酸进行甲酯化反应,考察了影响探头萃取效率的因素如时间,温度和盐浓度等,优化了衍生化条件.结果表明:该方法检测限低,重现性好,线性范围宽(2~3个数量级),回收率在78.38%~105.1%之间,可用于血清中游离脂肪酸的测定.     

激光烧蚀C60衍生物产生奇数碳笼团簇

利用激光烧蚀飞行时间质谱技术研究了Ｃ６０衍生物Ｃ６０ＣＨ２,Ｃ６０Ｒ２的Ｃ６０ＨＲ（Ｒ＝ＣＨ５ＣＯ－）的富勒烯团簇动力学,在负离子通道,对Ｃ６０ＣＨ２及Ｃ６０Ｒ２可清楚地观测到Ｃ５５＾－,Ｃ５７＾－等碳笼团簇离子,而对Ｃ６０ＨＲ虽然其正离子谱与Ｃ６０ＣＨ２和Ｃ６０Ｒ２相似,却观测不奇数碳笼团簇的产生。初步讨论了奇数碳笼团簇的产生及其与衍生物结构的关系。     

Study on fragmentation behavior of taxoids by tandem mass spectrometry

We have studied the fragmentation behavior of positive and negative ions of taxol and 6/8/6 type taxoids, the influence of different substituents on fragmentation, and the correlativity between fragmentation patterns and structure by MS/MS technique with different ionization methods such as FAB-MS, ESI-MS, etc. We have also investigated in detail the fragmentation of various molecular-related ions, such as [M+H]⁺, [M+Na]⁺ and [M-H]⁻ ions, and the formation pathways of characteristic fragment ions. It has been found that there exists some competing reaction between the loss of C-13 side chain and decomposition by loss of acetic acid. In addition, by comparing CID spectra obtained with low- and high-energy collision, it is seen that CID-MS/MS with low-energy collision is more suitable for the study of the structural analysis of small molecules and drug metabolites. The experimental results demonstrate that MS/MS spectra can reflect more effectively the slight difference of structure between the related compounds and their structural characteristic features than MS spectra, and can also provide a beneficial analysis basis for these kinds of compounds.     

流动注射在线分离富集-火焰原子吸收光谱法用于Cr(Ⅲ)和Cr(Ⅵ)的形态分析

在单阀流动注射系统中 ,分别以串联在阀体流路中的阴、阳离子交换树脂微型柱分离富集 ,两种洗脱剂逆向洗脱 ,实现了Cr(Ⅲ )和Cr(Ⅵ )的在线分离富集和火焰原子吸收光谱法同时测定 .当富集 2min时 ,分析速度为 1 8样 /h ,测定Cr(Ⅲ )和Cr(Ⅵ )的特征浓度分别为 1 0 .1 2 μg/L和 1 4.43μg/L ( 1 %吸收 ) ,线性范围分别为0～ 1 0 μg/mL和 0～ 1 5 μg/mL ,对浓度分别为 1 μg/mL的Cr(Ⅲ )和Cr(Ⅵ )测定的相对标准偏差分别为 1 .6 2 %和 3.94% .该法应用于实际水样分析 ,加标回收率在90 .9%～ 1 0 4 5 %之间 .     

氢化物发生原子荧光法测定土壤中铅镉砷3种有害重金属

应用氢化物发生-原子荧光法对土壤中铅镉砷含量进行测定。研究了分析测定条件;测定铅、镉、砷的线性范围分别为:0～40μg/L,0～5μg/L,0～40μg/L;相关系数分别为:0.9999,0.9999,0.9994。应用于样品测定,测定结果的相对偏差小于2.6%;加标回收率为96.8%～104%。     

胶束增敏荧光光度法测定阿莫西林的含量

研究发现,阳离子表面活性剂十六烷基三甲基溴化铵对阿莫西林的荧光有明显的增敏作用,据此建立了直接测定药片中阿莫西林含量的荧光光谱法.实验结果表明,阿莫西林的浓度在0.25～0.5和0.001～0.200mmol/L范围内与荧光度呈线性关系,检出限分别为34μmol/L和5.5μmol/L.该方法的回收率为99.6%～100.1%,相对标准偏差为0.16和0.18,用于阿莫西林样品的测定,结果令人满意.     

消解乳化技术-火焰原子光谱法测定天然橡胶中微量元素

在低温下用浓硝酸消解天然橡胶样品,以甲基异丁基酮溶解消解产物,并制成乳浊液.加入氯化锂溶液作为钠、钾的消电离剂及加入La3 作为钙、镁的释放剂.用火焰原子发射光谱法测定钠、钾、钙,以火焰原子吸收光谱法测定镁.建立了消解乳化技术-火焰原子光谱法测定天然橡胶中钠、钾、钙、镁的分析方法.对消解产物的溶解性质、溶剂及乳化剂的选择、试液与空白溶液物理性质的一致性,背景吸收干扰及检出限进行了考察.测定结果的相对标准偏差小于3.7%,加标回收率96.7%～104.7%.     

非完全消化-火焰原子吸收光谱法测定大米及小米中镁锌

以高氯酸 -硝酸 ( 1 + 3)混合酸作消解溶剂 ,用非完全消化处理样品 ,以火焰原子吸收法成功地测定了大米、小米中的镁、锌 .用Sr2 +作镁的释放剂以消除共存元素的化学干扰 .对样品处理条件、背景吸收干扰、试液与其空白溶液粘度的一致性、检出限及特征浓度进行了考察 .测定结果的相对标准偏差≤ 2 .1 % ,测定结果与灰化法一致 ,相对误差小于± 2 .1 % .在火焰原子吸收法中 ,用非完全消化法取代灰化法对大米、小米样品进行预处理是可行的 .     

质谱计的微机控制系统

给出了一个质谱计的微机控制系统,应用该系统,实现了对质谱计电离电压和质谱扫描的自动控制,根据质谱输出信号的大小自动选择最合适的测量量程,并可对质谱信号实时显示、存储保留及分析处理