气相色谱-质谱联用法分析北大仓白酒香气成分

利用溶剂萃取法进行分离和富集,采用气相色谱-质谱联用技术对北大仓白酒香气成分进行分析。从北大仓白酒的二氯甲烷萃取物中分离并鉴定了30种物质,其中酯类22种,占所有香气物质的94.847%;酸类2种,占4.659%;烷烃类2种,占0.228%;醇类2种,占0.185%;酮类1种,占0.060%;酸酐类1种,占0.021%。所含主要化合物为己酸乙酯、2-羟基丙酸乙酯和己酸,合计占总香气成分的96.396%,构成了北大仓白酒香气成分的骨架。     

4253例乙型肝炎病毒血清标志物定性结果模式分析

为适应乙肝两对半模式的变化,更准确地进行乙肝诊断,对4 253例乙型肝炎病毒血清标志物(HBVM)的结果模式特征进行了分析。采用ELISA法检测乙型肝炎病毒血清标志物(1-HBsAg、2-抗HBs、3-HBeAg、4-抗HBe、5-抗HBc)。结果表明,ELISA检测HBVM共得到18种模式,其中"全部阴性"占18.3%;"1、4、5阳性"比例最高占23.5%;"1、3、5阳性"占18.1%;"2阳性"占15.1%;"1、5阳性"占12.1%;"2、4、5阳性"占4.3%;"4、5阳性"占2.1%;"2、5阳性"占2.6%;"5阳性"占2.1%;其它特殊模式所占比例相对较低。     

茶叶中653种农药化学品残留GC-MS、GC-MS/MS与LC-MS/MS分析方法：国际AOAC方法评价预研究

选择了16个实验室,按AOAC方法评价指南对盲样进行了检测。对16个实验室的统计分析结果表明:剔除操作偏离方法的2个实验室的全部数据,剩余14个实验室GC-MS/SIM(GC-MS/MS):RSDr<8%的占100%;RSDR<16%的占57.5%,RSDR<25%的占92.5%;HorRat值小于1.0的占80.0%,HorRat值小于2.0的占97.5%。LC-MS/MS:RSDr<8%的占65.0%,RSDr<15%的占97.5%;RSDR<16%的占35.0%,RSDR<25%的占95.0%;HorRat值小于1.0的占92.5%,HorRat值小于2.0的占97.5%。建立的1 220条标准曲线中,有1 132个满足r2≥0.995的要求,占92.8%;检测目标农药离子3 600个,离子丰度符合EU要求的有3 443个,占95.6%。AOAC方法评价结果证明,该方法重现性和再现性良好,完全适用于茶叶中653农药残留的定性和定量分析。     

白云鄂博主矿霓石型稀土铁矿石中稀土元素在独立矿物中的富集状况研究

对白云鄂博主矿霓石型稀土铁矿石进行多元素分析,化验其元素组成及含量,并结合场发射电镜、能谱仪和自动矿物分析系统对其稀土富集状况进行了研究。结果表明:主矿霓石型稀土铁矿石稀土品位高达9.1%,轻稀土含量占稀土总量的97.91%,中重稀土含量占稀土总量的2.09%;稀土氧化物含量在氟碳钙铈矿中占元素总量的68.52%,在氟碳铈矿中占67.94%,在独居石中占61.66%,在黄河矿中占37.11%,在易解石中占28.33%;该类型矿石中稀土氧化物48.01%赋存于氟碳铈矿中, 21.21%赋存于独居石中, 7.34%赋存于黄河矿中, 5.87%赋存于氟碳钙铈矿中, 0.93%赋存于易解石中,这五种矿物稀土氧化物含量之和共占矿石中稀土总量的83.36%。     

痰热清的不良反应分析与用药指导

目的对痰热清药品不良反应监测报告的结果进行分析,为临床合理用药提供参考依据。方法对赣州市妇幼保健院2012—2014年使用痰热清后出现不良反应的288例患者进行分类统计,分析患者性别、年龄、联合用药情况、用药观察时间与不良反应的发生率和临床症状的关联性。结果在所有不良反应患者当中,男性患者占55.56%,女性患者占44.44%,年龄小于10岁占38.9%,年龄大于60岁占33.3%。在联用药物中,抗菌药的不良反应发生率占90%以上。用药后30 min内出现的不良反应占50%,用药后1 d内出现不良反应占22.2%;不良反应症状中,过敏反应占33.3%。结论痰热清的不良反应与患者的年龄、性别和联合用药情况有关,且发生时间多集中在30 min以内。不良反应的临床症状以过敏反应为主。     

苦碟子挥发油化学成分的分析

对我国东北地产苦碟子中挥发油成分进行系统分析,确定挥发油的化学成分,为阐述其生物活性提供依据.采用水蒸汽蒸馏法提取挥发油,气相色谱--质谱联用仪进行分析.结果鉴定出37种化合物.在这些化合物中,脂肪烷烃类占53.21%,酮、醛类占39.05%,烯、烯醇、烯酸类占4.94%,酯类占1.57%.其挥发油的主要成分是6,10,14-三甲基-2-十五烷酮,含量为33.98%.     

分子蒸馏分离废次烟末致香成分及在烟草中的应用

采用分子蒸馏技术对超临界CO₂萃取的废次烟末提取物进行分离,并对馏分进行GC-MS分析。 GC-MS结果显示,三级分子蒸馏(80、120、160 ℃)共鉴定出52种化学组分。 80 ℃轻组分段鉴定出15种,以杂环类为主,占总量的98.91%;其次为酯类,占总量的0.606%。 120 ℃轻组分段鉴定出26种,以杂环类为主,占总量的91.42%;其次为酮类、醇类和烃类,分别占总量的4.16%、2.87%和0.74%。 160 ℃轻组分段鉴定出26种,以醇类为主,占总量的67.97%;其次为杂环类,占总量的11.57%,烃类、醚类、酮类、酯类、醛类分别占总量的7.9%、4.09%、3.77%、2.80%、1.89%。 不同馏分段化合物种类和含量存在明显差异性,充分体现了分子蒸馏选择性富集的特点。 感官评吸表明,80 ℃轻组分和120 ℃轻组分按照质量比8:2调配后,香气质较好,香气量较足,口腔较舒适,有甜香显现,吸味较纯净,评吸结果较为理想。     

3671例少儿头发微量元素检测结果的分析

为掌握广州市某大型国有企业属下的幼儿园、小学、中学生微量元素状况,给微量元素缺乏病的临床诊断提供科学依据,对该企业的5所幼儿园、2所小学、1所中学的3 671例儿童进行了头发中元素钙、锌、铁、铜、锰、碘、铅的含量检测。结果表明,缺钙181人次,占4.9%;缺铁177人次,占4.8%;缺锌769人次,占20.9%;缺铜551人次,占15.0%;缺碘2 056人次,占56.0%;缺锰129人次,占3.5%;高铅2 668人次,占72.7%。提示幼儿园、小学生存在微量元素缺乏比例大,中学生除了碘、锰外大多数微量元素都不缺乏,无论是幼儿、小学生或中学生有害元素铅都偏高,是保健的重点。     

学龄前视力低常儿童散光眼分布特征分析

目的分析学龄前视力低常儿童散光眼分布特征,全面探究其散光类型、分布以及矫正情况,旨意为相关研究人员提供理论依据。方法选择2016年1月至2016年12月温州医科大学附属眼视光医院收治的912例学龄前视力低常者(1 730眼)为研究对象,实施散瞳验光,分析统计学结果。结果单眼散光者94例,占10.3%。双眼散光者818例,占89.7%。对称性散光者710例,占86.6%,不对称散光者108例,占13.2%。顺规散光1 646眼,占95.1%,逆规散光64眼,占3.7%,斜轴散光20眼,占1.2%。矫正视力在0.9以上者共计412眼,占23.8%。0.8以下共计1 318眼,占76.2%。在该部分群体中,远视性散光共计1 042眼,近视散光共计30眼。混合散光共计246眼。复性远视散光1188眼,占68.7%,复性近视散光38眼,占2.2%。单纯近视散光6眼,占0.4%,单纯远视散光204眼,占11.79%。混合散光294眼,占17.0%。0.50 D~1.00 D占31.7%,1.25 D~2.00 D占46.4%,2.25 D~3.00 D占15.6%,3.25 D~4.00 D占4.9%,4.25 D~5.00 D占1.3%。5.25 D以上占0.2%。结论在学龄前视力低常群体中,双眼散光为常见疾病类型,其中以复性远视散光为主。散光程度一般在3.00 D以下,轴向分布以顺规散光为主。重度散光为引发弱视的主要因素,因此对于视力低常学龄前儿童,应当做好早期视力筛查,以便尽早矫正散光,恢复正常视力。     

白马骨挥发油的GC-MS分析

采用水蒸气蒸馏法从白马骨中提取挥发油,再通过气-质联用(GC-MS)技术对所提取的挥发油的化学成分进行分离鉴定,共测定了其中的36种成分.已成功鉴定的成分占样品总量的93.39%,其主要成分为脂肪酸,占挥发油总量的74.23%,其次为烷烃化合物8.54%,酯类化合物3.96%,酮类化合物2.36%,烯烃化合物1.95%,醇类化合物1.71%,其它化合物(1个)仅占0.71%.     

油松籽油脂的提取及其脂肪酸组成与含量的评价

采用索氏提取法提取油松籽中的油脂,得油率为42.9%;对油脂进行甲酯化处理后用气相色谱-质谱联用仪检测其中的脂肪酸组成及含量。实验结果表明,油松籽油中含有7种脂肪酸,分别为肉豆蔻酸10.38%、硬脂酸3.05%、油酸21.98%、亚油酸(13,16-十八碳二烯酸)3.53%、亚油酸(9,12-十八碳二烯酸)38.38%、亚麻酸20.06%和二十碳三烯酸2.62%,其中饱和脂肪酸含量为13%,不饱和脂肪酸含量为87%。     

GC Analysis of the Fatty Acid Composition of Yak Kidney

To obtain valuable information for development of potential commercial products from yak kidney, which is usually treated as waste, the fatty acid composition of kidneys from yak reared in Gansu province, China, was investigated by gas chromatography. Fifteen different fatty acids were identified. The major fatty acids are oleic acid (33.3%), stearic acid (20.2%), and palmitic acid (18.4%). More interestingly, several important and essential fatty acids were also identified, including conjugated linoleic acid (2.94%), omega-3 fatty acids, for example docosahexaenoic acid (1.47%), eicosapentaenoic acid (1.11%) and alpha linolenic acid (0.37%), and omega-6 fatty acids, for example arachidonic acid (2.86%) and linoleic acid (1.98%). The results show that the fatty acid composition of yak kidney is of reasonable value and is suitable for further development of possible commercial products. This is the first report of the fatty acid profile of yak kidney.

     

柽柳实中挥发油和脂肪酸分析

首次研究了维药细穗柽柳(Tamarix leptostachys Bunge)实中挥发油和脂肪酸的化学成分。 分别采用药典中的挥发油提取法和索式取提法提取柽柳实中的挥发油和脂肪酸,使用气质联用技术获取总离子流图,各色谱峰相应的质谱图经过NIST2011标准谱库检索定性,并采用峰面积归一化法进行定量分析,计算各成分的相对百分含量。 两种方法分别鉴定出48种挥发油和19种脂肪酸。 挥发油主要成分为芳香类化合物(43.71%)、芳香性醛酮类(20.58%)、脂肪酸类(13.03%)、酯类(17.36%)和醇类(4.19%)等。 脂肪酸主要成分为棕榈酸(35.61%)、亚油酸(27.26%)和油酸(11.33%)等,其中不饱和脂肪酸含量占总脂肪酸含量的38.65%。 维药细穗柽柳实中富含丰富的挥发油和不饱和脂肪酸,具有很好的开发利用价值。     

用GC-MS法分析柿树叶中的脂肪酸

用乙醚－己烷混合溶剂抽提柿树叶中的脂肪酸,ＮａＯＨ－ＣＨ３ＯＨ交换法甲酯化,毛细管柱ＦＦＡＰ作为分离柱,进行气相色谱－质谱法测定脂肪酸（以甲酯的形式）的组成。共分离出２１种脂肪酸,鉴定出１９种,占总含量的９８．７２％,其中以肉豆蔻酸（６．６８％）、棕榈酸（３０．００％）、硬脂酸（１０．４２％）、十六碳三烯酸（１．４４％）、亚油酸（１．８４％）、十八碳－烯酸（２２．２２％）、亚麻酸（１．２５％）、花     

Evaluation of oil content and fatty acid composition of five endemic Bupleurum species growing in the Central Anatolia region of Turkey

The fatty acid composition of five endemic Bupleurum (Apiaceae) species was analysed by GC technique for their nutritional value. The amount of oil content of the species varied from 3.77% to 7.03%. Twenty-one fatty acids were identified in the oils. The fatty acid composition of the studied species contained oleic, palmitic and linoleic acids as the major components. Oleic acid ranged from 8.81% to 68.30%, while the levels of palmitic acid were found to be between 12.47% and 47.85%. Bupleurum lycaonicum, Bupleurum sulphureum and Bupleurum heldreichii are very good sources of oleic acid. The remaining species were characterised as containing the highest level of palmitic acid. In this study, the total saturated fatty acids ranged between 15.02 and 65.20%, while total monounsaturated fatty acids were between 18.10 and 70.65%. The total polyunsaturated fatty acid accounted for 13.47-35.20% of the studied fatty acids. Therefore, we can conclude that Bupleurum oils have a significant nutritional value.     

Determination of halogenated acetic acids and 2,2-dichloropropionic acid in water samples

Summary A new method is described for the determination of halogenated acetic acids and 2,2-dichloropropionic acid in slightly polluted water. The acids were extracted in a light-phase rotary perforator, derivatised with diazomethane and determined by GC-ECD and GC-MS. The standard deviations were in the range of 14.5–16.8%. Average recoveries were 82%, 92% and 79% for monochloro-, dichloro- and trichloroacetic acid, respectively. The extraction yields for the bromoacetic acids and dichloropropionic acid were in the range of 64–85%.     

固相萃取-高效液相色谱法测定蜂蜜中的有机酸

建立了固相萃取-高效液相色谱(SPE-HPLC)同时测定蜂蜜中5种有机酸(L-苹果酸、马来酸、琥珀酸、柠檬酸、D-苹果酸)含量的方法。蜂蜜经制样后过Bond Elutes SAX固相萃取(SPE)小柱净化,用C18-MS-II反相色谱柱(250 mm×4.6 mm, 5 μm)进行分离,流动相为2%偏磷酸溶液,流速为0.7 mL/min,检测波长为210 nm。在此条件下5种有机酸在相应的线性范围内其线性相关系数均大于0.9967;方法的回收率为86.0%～103.9%,相对标准偏差为5.7%～9.8%(n=6),检出限为0.06～9.4 mg/kg。所建立的方法可用于蜂蜜样品中有机酸的测定。     

Analytical Characterization of Fatty Acids Composition of Bioactive Stem Oil of Maytenus royleanus by Gas Chromatography Mass Spectrometry

The significant inhibition and selectivity for human solid tumor cell by oily fraction of Maytenus royleanus, was subjected to GC‐MS analysis for determination of its chemical constituents. GC‐MS profile of methyl ester derivatives of fatty acids, showed that Palmitic acid (35.41%), Oleic acid (10.91%), Stearic acid (5.31%), Margaric acid (5.13%), Behenic acid (5.18%) and Hexanoic acid (4.97%) were the major components in the isolated oily fraction, while rest of the other fatty acids were present in minor concentration. The literature revealed that no such work has been done for the determination of fatty acids in M. royleanus stem oil.     

Contribution to the analysis of the essential oil of Helichrysum italicum (Roth) G. Don. Determination of ester bonded acids and phenols

The essential oil of Helichrysum italicum (Roth) G. Don (everlasting or Immortelle essential oil) was isolated by hydrodistillation and analysed by GC and GCMS. Forty four compounds were identified. The main components were alpha-pinene(12.8%), 2-methyl-cyclohexyl pentanoate (11.1 %), neryl acetate (10.4%), 1,7-di-epi-alpha-cedrene (6.8%) and other compounds. The oil was fractionated and ester-containing fraction was hydrolysed with KOH/H(2)SO(4). The liberated volatiles were analysed by GC and GC-MS: three phenols and twenty seven volatile carboxylic acids were identified[70% low fatty acids (C(2)-C(5)), 15% C(10)-C(12) acids and 15% other acids]. The main acids were acetic acid (24.3%) propanoic acid (17.2%), 2-methylpropanoic acid (11.4%),dodecanoic acid (8.7%), 2-methylbutanoic acid (8.3%), (Z)-2-methylbutenoic acid(5.1%) and decanoic acid (4.6%). With respect to the identified bonded carboxylic acids,the minimal number of esters in the oil was twenty seven, but their overall quantity was probably larger due to different possible combinations of alcohols with acids to form esters. On the other hand, only six main esters were identified in the oil before fractionation and hydrolysis.     

马齿苋及其籽中脂肪酸的比较研究

本实验利用ＧＣ－ＭＳ分析技术对马齿苋全草及其籽中的脂肪酸（以甲酯的形式）进行了分析，共鉴定出８种脂肪酸。全草中以亚麻酸（４７．１６％）、亚油酸（２２．００％）及棕榈酸（１７．４％）为主，籽中以亚油酸（４５．８６％）及亚麻酸（３０．６１％）为主。