气相色谱-质谱(GC-MS)联用法分析当归挥发油中化学成分

当归是名贵中药,挥发油是当归的主要活性成分。本文采用水蒸气蒸馏法提取当归挥发油,用气相色谱-质谱联用(GC-MS)法定性定量分析了当归根的挥发油。通过质谱库检索得到其中41个组分的定性定量结果,占挥发油总含量的93.65%。     

气相色谱法用于甲醇氧化转化率的研究

采用GDX 5 0 2为固定相 ,用GC色谱法对常温常压下甲醇氧化为甲醛的转化率进行监测。找出了分离测定甲醇、甲醛、水、甲酸、乙醇等物质的优惠色谱条件。该法灵敏度高 ,甲醇的最小检测量为 9 2 6× 10 - 7g。考察了氧化剂的种类、用量、介质的选择和氧化时间的长短、温度、溶剂等因素对甲醇氧化转化率的影响 ,得到了优惠反应条件。结果表明 :常温常压下 ,不采用任何催化甲醇氧化转化率可达 72 38% ,甲醛回收率为 92 0 8%。     

Simultaneous determination of adenine, uridine and adenosine in cordyceps sinensis and its substitutes by LC／ESI-MS

A simple, sensitive and reproducible high performance liquid chromatography-mass spectrometry coupled with electrospray ionization method for simultaneous separation and determination of adenine, adenosine and uridine was developed. The analytical column is a 2.0 mm× 150 mm Shimadzu VP-ODS column and volume fraction of the mobile phase is 86.5 %water, 12.0%methanol and 1.5%formic acid. 2-chloroadenosine was used as internal standard. Selective ion monitoring mode and selective ion monitoring ions at ratio of mass to electric charge of 136 for adenine, 268 for adenosine and 267 for uridine were chosen for quantitative analysis of the three active components. The results show that the regression equations and linear range are Y=0. 062X 0. 005 and 2.0 - 140.0μg · mL 1for adenine, Y=0. 049X 0. 004 and 4. 0 - 115.0 μg · mL-1 for uridine, Y=0. 154X 0. 014 and 1.0 - 125.0 μg · mL 1 for adenosine. The limits of detection are 0.6 μg · mL 1 for adenine, 1.0μg · mL-1 for uri dine and 0.2 μg · mL 1 for adenosine.The recoveries of the three constituents are from 96.6% to 103.2%.     

Determination of constituents of essential oil from Angelica sinensis by gas chromatographymass spectrometry

1INTRODUCTION TraditionalChinesemedicines(TCMs)are veryimportantduetotheirextensiveuseinpre ventingandcuringmanydiseasesforhumans.Al thoughonlysomecompoundsmightberesponsible forpharmaceuticaleffects,traditionalChinese medicinesusuallycontaintoomanycomponentsandformaverycomplexsystem,whichmakesthe screeningandanalysisofbioactivecomponentsex tremelydifficult[1]comparedwiththoseofwesternmedicines.Whensuchcomplexsamplesareana lyzed,itiscommonthatdifferentcontentsof multi componentsandgreatd…     

废水中甲胺磷的快速测定及处理

以薄层—碘量法 ,钠氏试剂法和气相色谱法三种方法对甲胺磷的含量进行了测定。以气相色谱法作为对照 ,采用活性炭、阳离子交换树脂、GDX 5 0 2和灰煤等四种物质处理甲胺磷废水 ,选择了最佳处理方案 ,废水中甲胺磷的去除率达 90 %以上。     

烟用香精香气成分提取方法的选择

采用同时蒸馏萃取、水蒸气蒸馏、固相微萃取和溶剂萃取法分别提取烟用香精中的挥发性成分,并采用GC和GC/MS进行测定,通过比较色谱指纹图谱中提取特征组分的数目、含量和表征香精指纹性的能力,以及提取方法的重复性,得到其最佳提取方法。结果表明:同时蒸馏萃取法能最大程度提取AB1香精样品的风味成分并具有较好的重复性,可以满足建立指纹图谱的要求。     

Heavy metals accumulation effect in rabbit body fluids after smoking

Concentration of heavy metals in blood and urine of rabbit after inhaling three different kinds of cigarette was studied through the animal passive smoking pattern. The samples were prepared by nitric acid solution digestion and determination of seven kinds of heavy metals including Hg, Se, Sn, Pb, Cd, Ni and Cr was performed by inductively coupled plasma-atomic emission spectrometry (ICP-AES). The ICP-AES method was established with good precision and accuracy, relative standard deviation (n=6) was between 2.9% and 5.9%, and the recovery was in the range of 95.0%–104.2%. Concentration of six heavy metals increases in some extent in blood and urine after period of smoking and the increasing of heavy metals in blood and urine all shows time dependence. Significantly higher heavy metal levels are observed in the blood and urine of the cigarette inhaling rabbits in the exposed group. The concentration of six kinds of heavy metals in the blood of the rabbit increases after 16 weeks exposing to cigarette smoking. Three times of Hg, ten times of Se and trace amount of Pb, Cd, Ni and Cr are detected in the blood after 16 weeks of smoking. For urine samples, about three times of Hg, two times of Se, five times of Pb and trace amount of Cd are detected after 16 weeks of inhalation of cigarette. Comparatively, higher concentration of heavy metals are detected after inhaling of Nise cigarette.     

氢化物发生-ICP-AES联用测定蔬菜中微量的砷的含量

选用氢化物发生器和ICP-AES进行联用技术,测定蔬菜中微量的As的含量,首先对仪器条件进行优化,然后对消解体系以及消解液的用量,酸介质浓度,NaBH4浓度,预还原剂的用量以及放置时间,共存元素的干扰进行考察,确定了最佳的实验方案。该方法简单,快速,准确度高,该方法的检出限为:0.0003 mg/L,测定空白溶液10次的RSD为6.62%,测定蔬菜样品的回收率在90%～106.4%之间,适合蔬菜中低含量的As的测定。     

橙皮苷分析方法研究

以橙皮苷为标准品,采用紫外分光光度法(直接法)和高效液相色谱(HPLC)测定橙皮苷含量,并对测定条件进行探讨,比较两种方法测定橙皮苷的准确度。实验结果表明,紫外分光光度法测得的橙皮苷纯度数据比高效液相色谱数据高,HPLC法精确,分光光度法简单快速,均能得到令人满意的结果。     

2-羟基-6-萘甲酸及其杂质含量的液相色谱测定

用甲醇-乙腈和0.02 mol/L KH2PO4溶液为流动相进行梯度洗脱,在AKsail ODS色谱柱建立了分离检测2-羟基-6-萘甲酸及其杂质的分析方法。结果表明,2-羟基-6-萘甲酸、2-萘磺酸、1,4-萘二甲酸、2-羟基-6-萘甲酸甲酯、2-羟基-3-萘甲酸的RSD分别为0.000 4%、0.14%、0.23%、0.08%、0.11%,回收率为86.70%～100.5%,定量限、线性关系、精密度和加标回收率均能满足定量分析要求。