826例儿童发铅、锌、铜、铁、钙含量分析

探讨了东乡县儿童体内微量元素情况。对826例儿童发铅、锌、铜、铁、钙检测结果分各年龄组进行了分析。结果表明,826例儿童中发铅含量超标512例,占61．99％;发锌含量低标604例,占73．1％;发铜含量低标46例,占5．6％;发铁含量低标95例,占11．5％;发钙含量低标116例,占19．6％,占19．6％。5种元素含量与年龄有关,随着年龄增大,发铅、锌、铜、钙含量下降,发铁含量上升。分析表明,儿童铅污染、锌、钙缺乏程度相当普遍且严重。在儿童生长发育期进行常规的微量元素检测非常必要。     

气相色谱法测定冠心膏中樟脑、薄荷脑、异龙脑、龙脑的含量

用气相色谱法测定了冠心膏中樟脑、薄荷脑、异龙脑和龙脑的含量。固定相：７％ＰＥＧ－１５００,线性范围：５～４５０ｍｇ／Ｌ（ｒ＝０．９９９４～０．９９９９）。回收率：樟脑为９８．４４％,薄荷脑为９９．０１％,异龙脑为９９．６９％,龙脑为１０１．９％。     

马兰菜中的营养元素

采用原子吸收分光光度法对马兰菜中的营养元素进行了分析。结果表明马兰菜中营养元素含量丰富,与一般蔬菜比较,其Ｓｅ,Ｚｎ,Ｍｇ,Ｃａ含量更高。但热风脱水处理后,其Ｓｅ,Ｖ含量则减少,且地域不同其微量元素含量有所不同,采用标准加入法进行考察,回收率为９３．３％￣１０６．７％,结果满意。     

不同区域儿童血铅浓度及铅危害的防治

实验选择了生活在杭州市区５￣６岁学龄前儿童１２０名，男女各半，并选择了生活在杭州近郊海查市农村同龄儿童１００名为观察对照组，进行了血铅含量的测试。结果显示，生活在杭州市中心的儿童受到铅污染的危害程度比生活在农村的儿童较为严重。以目前公认推荐血铅可接受上限值０．４８３μｍｏｌ／Ｌ计算，杭州市有４９．１％、而海宁农村有３１．９％的儿童血铅浓度超过允许标准。儿童的严重铅危害，应引起人们高度重视。     

空气－C_2H_2火焰原子吸收光谱法测定中草药（鸦胆子、补骨脂）中的铁、锰

用空气－Ｃ２Ｈ２火焰原子吸收光谱法测定了中草药（鸦胆子、补骨脂）中的Ｆｅ、Ｍｇ含量，讨论了测定条件，结果令人满意，方法的回收率：Ｆｅ９８．２０％～１０４．９％，ＣＶ＝１．０６％～１．０７％，Ｍｎ９９．４％～１０１％，ＣＶ＝０．５２％～１．９４％。     

絮凝剂中铝、砷、镉、汞、锰和铅的测定

1 引 言聚合硫酸铝是一种新型絮凝剂，可以用作污水处理。一般固铝含量为１０％～３０％，Ａｓ、Ｃｄ、Ｈｇ、Ｍｎ、Ｐｂ的含量为ｎｇ～ｍｇ／Ｌ级。通常测定这些元素的方法为分光光度法、原子吸收法、滴定法、原子荧光法等。这些方法对于聚合硫酸铝来讲，有的达不到测定灵敏度，有的基体干扰严重，有的前处理繁琐、费力，有的测定费时，并且大多数方法不能同时测定多元素。以等离子体质谱法测定絮凝剂聚合硫酸铝中的６种有毒元素Ａｌ、Ａｓ、Ｃｄ、Ｈｇ、Ｍｎ、Ｐｈ含量，测定准确度分别为9７．０％、１０４％、８８．４％、９２．８％、９…     

1～7岁儿童309例发铁观察

１～７岁儿童发铁检查３０９例，其中血红蛋白正常范围１３２例，血红蛋白９～１２ｇ％１７７例．血红蛋白正常范围组，发铁低于正常值占２６．５％，有部分儿童存在非贫血型铁缺乏．血红蛋白９～１２ｇ％组，发铁低于正常值占１９．７％．血红蛋白下降的儿童，仅部分是铁元素缺乏引起．铁元素缺乏的发病率，两组相比，无显著性差异（Ｐ＞０．０５）     

256名7～14岁儿童头发锌、铜、铁、钙含量及分析

测定株洲市东区４个单位的２５６名儿童头发中锌、铜、铁、钙含量．结果发锌平均值为１５０．７５×１０－６，发铜９．７６×１０－６，发铁４５．９３×１０－６，发钙４８１．３１×１０－６．结果表明儿童期各年龄组间，男、女性别间差异无显著意义。     

4776例儿童头发锌、铜含量的回顾性评价

对４７７６例９个月至４岁儿童发锌,铜含量进行了检测分析,发现有半数以上儿童发锌降低,约三分之一儿童发铜减少。     

水果、蔬菜中16种有机氯残留农药的毛细管气相色谱测定法

采用柱层析净化方式,以ＨＰ－１０１弹性石英毛细管柱为分离柱,电子捕获检测的气相色谱法测定水果、蔬菜中１６种有机氯农药残留量。方法的检出限为０．１×１０－９～２．０×１０－９,回收率范围在８７．５％～１０６．３％之间,相对标准偏差为３．０％～９．５％。     

基于MALDI质谱成像技术分析莲子中代谢物的组织分布

该文建立了一种可对莲子中多种代谢物进行高覆盖分析的基质辅助激光解吸附质谱成像(MALDI-MSI)方法,实现了莲子中生物碱类、黄酮类、氨基酸类、脂肪酸类、有机酸类、胆碱类、磷脂类等多种代谢物的组织原位可视化表征。结果表明,生物碱类代谢物主要分布在莲子胚芽中;黄酮类代谢物主要分布在莲子胚芽和种皮中;氨基酸类代谢物在莲子子叶中的含量显著高于莲子胚中;脂肪酸类代谢物在莲子不同组织中的分布差异很小;胆碱类代谢物在莲子胚芽和莲子子叶底部的含量更高,甘油磷酸胆碱在莲子子叶顶部的含量更高;有机酸类代谢物以及绝大多数磷脂类化合物在莲子子叶中的含量高于莲子胚。该研究为评价莲子药物质量、探究莲子中化合物的时-空代谢网络提供了新的技术支持。     

Structural,Pasting, and Thermal Properties of Ultra-high Pressure-treated Lotus Seed Starch

Lotus seed starch(15%, w/w) was subjected to ultra-high pressure(UHP) at 500 MPa for 10~60 min. The effects of UHP on the structural, pasting, and thermal properties of starch were investigated using solid-state 13C CP/MAS NMR, differential scanning calorimetry(DSC), HPSEC-MALLS-RI, and a rapid visco analyzer. The 13C CP/MAS NMR results revealed a reduction in the relative crystallinity and peak intensity of the crystalline state with increasing the UHP time. The molecular weight of native starch was 1.433 × 107 Da, which was higher than that of the UHP-treated starch. Viscograms of UHP-treated starch revealed an increase in paste viscosity, peak time, and pasting temperature and a reduction in breakdown and setback viscosity compared to the native starch. Furthermore, the DSC results showed a reduction in gelatinization temperature and gelatinization enthalpy with increasing the UHP time.     

Determination of Lotus Leaf Alkaloids by Solid Phase Extraction Combined with High Performance Liquid Chromatography with Diode Array and Tandem Mass Spectrometry Detection

Lotus (nelumbo) is a traditional Chinese medical herb, and alkaloids are responsible for its pharmaceutical activities. Therefore, a rapid, validated method to determine alkaloids in lotus leaves is useful for its quality control. The goal of this work was to develop and validate an analytical method for the identification and quantitation of the bioactive alkaloids of extracts from lotus leaf and classification of lotus germplasm based on alkaloid concentrations. Solid-phase extraction was used prior to high-performance liquid chromatography coupled with photodiode array detection at 272 nm and tandem electrospray ionization triple quadrupole mass spectrometry for analysis. Nuciferine and O-nornuciferine were the dominant compounds in lotus used for seed production and some used for flower production. However, anonaine, roemerine, and N-nornuciferine were abundant only in some lotus flowers. All the lotuses were classified into four groups by principal component analysis of alkaloid content: 10 flower and three seed lotuses characterized by high nuciferine and O-nornuciferine content; 12 flower lotuses with high N-nornuciferine, roemerine, and anonaine content; two flower lotuses with a relatively high content of all five alkaloids; and cultivars with a low alkaloid content and without dominant alkaloids.     

QuEChERS与液相色谱-串联质谱联用检测中药、调味品及外敷药物中去甲乌药碱的含量

针对中药材、调味品及外敷药物中的去甲乌药碱,建立了一种基于QuEChERS前处理与液相色谱-串联质谱（LC-MS/MS）联用的检测新方法。样品经甲酸-乙醇提取、QuEChERS吸附剂净化后,样品溶液引入LC-MS/MS进行分析,在多反应监测模式下检测。该方法的检出限为0.03 ng/g,线性范围为0.10~100 ng/g,精密度为4.33%（0.50 ng/g,n=7）。采用所建立的方法对市售的13种中药、4种调味料及1种藏药贴膏中的去甲乌药碱含量进行了检测,在干荷叶、干莲子、山药、玉竹、淮山、花椒、桂皮及骨痛贴膏中检出去甲乌药碱,其含量分别为9667.6、1183.8、21.5、8.2、8.5、148.6、21.3、173.3 μg/kg。对花椒和桂皮进行加标回收试验,回收率在92.6%~109.8%之间,表明所建立的方法具有良好的准确性。综上,该方法具有快速、简便、可靠、可批处理的优点。     

固相萃取-液相色谱-串联质谱法测定莲蓉馅料中的二氧化硫脲

建立了固相萃取-液相色谱-串联质谱法测定莲蓉馅料中违法添加的二氧化硫脲的分析方法。采用0.05%(v/v)醋酸溶液从馅料中提取二氧化硫脲,经BOND ELUT PLEXA固相萃取柱(60 mg/3 mL)净化,采用Agilent亲水作用色谱柱(100 mm×2.1 mm,3.5 μm)分离,以0.01 mol/L醋酸铵(冰醋酸调pH至3.5)和乙腈为流动相,在多反应监测模式(MRM)下进行定性定量分析。最终,二氧化硫脲在10~1000 μg/L范围内线性关系良好,检出限(LOD)和定量限(LOQ)分别为8.0 μg/kg和30.0 μg/kg,方法回收率为75.3%~80.7%,相对标准偏差(n=6)不超过4.83%。此方法快速、准确、特异性强、灵敏度高、样品前处理方法简便易行,适用于莲蓉馅料中二氧化硫脲的确证与测定。     

磷肥和有机肥对莲藕根状茎品质和铁膜形成的影响

以莲藕为材料,研究了施用磷肥和有机肥及两者混施对莲藕根状茎品质和表面铁膜形成的影响,以期为高产优质莲藕的种植提供理论依据。结果表明,磷肥处理后莲藕根状茎中蛋白质和淀粉含量分别比对照增加了145．4％和61．5％,并且还原糖含量和维生素C含量也比对照提高了48．2％和112．7％,根状茎表面铁膜的铁含量显著低于对照。有机肥处理下蛋白质和还原糖含量分别比对照提高了54．0％和47.2％,但莲藕根状茎中的淀粉、维生素含量以及铁膜的产生与对照无显著差异。磷肥＋有机肥处理的效果仅次于磷肥。可见磷肥施用后有效提高了莲藕品质并减轻了根状茎表面铁膜沉积,这对于提高种藕效益具有非常重要意义。     

Studies on the Alkaloids of Lotus Receptacle

From lotus receptacle (seed pod of Nelumbo nucifera Gaertn., four alkaloids, nuciferine (I), N-nornuciferine (VIII), oxoushinsunine (IX) and N-norarmepavine (X) were isolated. Identification of these bases were carried out by their spectral data and direct comparison with authentic samples. It is interesting that oxoushinsunine (IX), a cytotoxic alkaloid shows tumor inhibitory activity against nasopharynx carcinoma reported recently by D. Warthen et al¹³⁾. The biscoclaurine (IV and V) and quaternary water soluble base (VI) only occures in the embryo. Comparison their alkaloids distribution in each part of Formosan lotus was listed in the Table 1.     

Comparison of sample preparation methods combined with gas chromatography with electron‐capture detection for the analysis of multipesticide residues in lotus seeds

Sample preparation is always the major bottleneck in analytical chemistry for the determination of pesticide residues. Different sample preparation methods have been proposed due to the wide variety of pesticides used and the inherent complexity of the matrices. In this study, different sample preparation methods including SPE, matrix solid‐phase dispersion, the quick, easy, cheap, efficient, rugged, and safe method, and a one‐step completion method were compared and evaluated for extracting pesticides from lotus seeds. Analysis was carried out using GC with electron‐capture detection. The results showed that good recoveries for tested pesticides were obtained by using Florisil in the four methods, and the extraction efficiency of the one‐step completion method was superior to the other three methods. The one‐step completion method was confirmed to have good linearity, reproducibility, stability, and recovery for the detection of 36 pesticides in lotus seed samples. The data collected from this study are expected to prove useful in regulating the concentration of the residues in lotus seeds, as well as in protecting human health from the hazards posed by these residues.     

On the Alkaloids of Nelumbo Nucifera Gaertn. Studies on the Alkaloids of Loti Embryo

A new tertiary tetrahydroisoquinoline alkaloid, methylcorypalline (V) and biscoclaurine base, neferine (II) were isolated from a Formosan lotus embryo (embryo of the seed of Nelumbo nucifera Gaertn.) (Nymphaeaceae), besides the earlier reported isoliensinine (I) and lotusine (IV). Characterization of this new base, methylcorypalline (I), mp. 58–59° (n-hexane), , by spectral data and direct comparison with synthetic sample prepared from vanillin have proved to be 6,7-dimethoxy-2-methyl-1,2,3,4-tetrahydroisoquinoline (V). Methylcorypalline (V) is the first instance occurring in nature having coronary dilator action.