HPLC-UV测定红酒中7种黄酮苷元及其生物活性物

建立了三元梯度的高效液相色谱法(HPLC)测定红酒中的桑色素、槲皮素,山奈酚、异鼠李素、木犀草素、芹菜素等苷元的含量的方法。采用Luna C18(4.6mm×150mm,3μm)色谱柱,预柱(4mm×3.0mm),柱温为50℃,流动相:A相乙腈,B相乙醇,C相为0.2%磷酸水溶液。流速为0.25mL/min,梯度淋洗,检测波长265nm。结果显示:各黄酮苷元在0.7mg/L~32.0mg/L呈线性关系,样品的加标平均回收率为98.2%~101.1%,RSD为1.88%~2.85%,该方法简便、准确,可用于天然产物中黄酮苷元的含量的测定。     

超高效液相色谱法测定不同产地桑叶中4种主要黄酮含量

目的建立超高效液相色谱(ultra performance liquid chromatography, UPLC)测定桑叶中4种主要黄酮含量的方法,并通过主成分和热图分析比较10个不同产地桑叶中4种黄酮含量的差异。方法选择ACQUITY UPLC BEH C₁₈为色谱柱(2.1 mm×50 mm, 1.7μm),甲醇溶液和0.5%磷酸溶液分别作为流动相A和B进行梯度洗脱。检测波长设置为350 nm;柱温设置为30℃。采用TB tools软件进行主成分分析和热图分析。结果 4种黄酮对照品在相应浓度范围内均呈良好的线性关系(r>0.999);回收率为98%~102%,相对标准偏差为1.12%~1.86%。且10个产地桑叶4种黄酮含量差异较大,具体表现为:安徽地区桑叶中芦丁、异槲皮苷、紫云英苷和槲皮素含量均最高,分别为20.543、6.801、1.328、3.645 mg/g;湖南桑叶中异槲皮苷的含量最低,为3.902 mg/g;其余3种黄酮化合物均在河北地区含量最低,分别为芦丁10.021 mg/g、紫云英苷0.348 mg/g和槲皮素1.784 mg/g。主成分和聚类分析结果显示,桑叶具有明显的地域差异性。结论该方法操作简单,分析时间短,稳定性强,可大大降低分析成本,且不同产地桑叶质量差异明显,可作为桑叶用药来源选择的参考。     

HPLC法测定酒萸肉中马钱苷含量

目的 建立高效液相色谱法测定酒萸肉中马钱苷含量方法.方法 色谱柱Agilent C18柱 (4.6mm×150mm,5μm);流动相乙腈-水(15:85);检测波长240nm;流速1.0ml·min-1;结果马钱苷在5～50μg·mL-1的浓度范围内具有良好的线性关系(r=0.9995).回收率为97.73%,RSD=0.48%.结论 该方法简便、可靠、准确,可用于测定酒萸肉中马钱苷含量.同时暂定酒萸肉中马钱苷含量限度不得低于0.60%.     

不同采收期大花罗布麻叶中黄酮类成分含量的测定

建立大花罗布麻叶中黄酮类成分槲皮素、芦丁、金丝桃苷的高效液相色谱-串联质谱（HPLC-MS/MS）测定方法,分析不同采收期的大花罗布麻叶中这3种黄酮类成分的变化。结果表明,芦丁在大花罗布麻叶的整个生长期中均未检出;槲皮素在10月份有检出,其他月份无检出;金丝桃苷整个生长期中均有检出,其中6～8月含量较高,故适宜采收期为6～8月;该检测方法加标回收率为98.0%～102.3%,相对标准偏差（RSD）为1.44%～2.63%,在各自的浓度范围内线性关系良好。高效液相色谱-串联质谱法可用于大花罗布麻叶中3种黄酮类成分的含量测定。     

高效液相色谱法快速测定大豆异黄酮制品中有效成分的研究

采用高效液相色谱法测定大豆异黄酮制品中染料木苷、黄豆苷、染料木黄酮和黄豆苷元含量.固定相为Agilent-1100 C18柱(3.9 x 150mm);以甲醇:水=35%～45%为流动相,进行梯度洗脱,流速为1.0～2.0mL/min;柱温为室温;检测波长为260nm.实验结果表明,市售30%大豆异黄酮制品中,含大豆异黄酮糖苷近28%,其中染料木苷为4%、黄豆苷为8%,苷元形式异黄酮未检出;采用酶水解法制备的大豆异黄酮水解物中含染料木黄酮14.3%、黄豆苷元9.8%,其大豆异黄酮苷元占大豆异黄酮总含量的96%.     

高效液相色谱法同时测定大豆粕四种异黄酮含量研究

该文介绍高效液相色谱同时测定大豆粕中四种大豆异黄酮方法。确定出色谱条件为:色谱柱Hypersil ODS2C18柱(250min×4．6mm ID,5μm),流动相:甲醇:水=40:60,柱温30℃,流速1．0ml／min,检测波长260 nm。大豆苷、染料木苷、大豆苷元、染料木素在0．21-8．56μg／mL范围内浓度与峰面积具有很好线性关系,相关系数r=0．999155-0．999991;该测定法回收率大于99％,变异系数小于3％。     

HPLC同时测定女金片中3种成分的含量

目的 建立高效液相色谱法,同时测定女金片中芍药苷、橙皮苷和黄芩苷的含量.方法 色谱柱:Eclipse Plus C18(5μm,4.6 mm×250 mm);检测波长:230,280 nm;流动相:乙腈-0.05％磷酸溶液,梯度洗脱;柱温:30℃;流速:1.0 ml/min;进样体积:10μl.结果 芍药苷浓度在6.0...     

利用高效液相色谱法测定甜茶叶中甜茶苷含量方法的研究

本文建立一种采用高效液相色谱测定甜茶叶中甜茶苷含量的方法。依据试验结果,甜茶苷测定前处理过程中,以30%乙腈溶液为溶剂,采用超声方式对甜茶叶进行处理能获得最佳的甜茶苷提取率。色谱条件:C_(18)柱(250mm×4.6mm×5μm);流动相:0.05%磷酸溶液-乙腈(68+32);流速:1mL/min;检测波长:210 nm;进样量:5μL;柱温:40℃;外标法定量。在该色谱条件下,甜茶苷浓度为0mg/mL～1.5mg/mL的范围内,甜茶苷峰面积(Y)与甜茶苷浓度(X)具有良好的线性关系,线性回归方程Y=21.0844X,相关系数r=1.0000;加标回收率为96.2%～102.3%;精密度(RSD)为1.23%。相关试验数据证明,该方法快速简单、重复性好、准确,适用于甜茶叶中甜茶苷含量的测定。     

HPLC法同时测定蓝莓汁及其发酵酒中9种有机酸

采用高效液相色谱法测定蓝莓汁及其发酵酒中有机酸含量。色谱条件为:色谱柱:Waters symmetry C1 8(4.6mm×250mm,5μm);流动相:NH4H2PO4(4g/100mL)溶液(磷酸调pH值为2.0);流速:1.0mL/min;检测波长:210nm;柱温:室温。通过该方法检测蓝莓汁及其发酵酒中9种主要有机酸:草酸、酒石酸、苹果酸、异柠檬酸、莽草酸、乳酸、乙酸、柠檬酸、琥珀酸,其平均回收率为99.52%,平均相对标准偏差为0.019%。     

高效液相色谱法测定不同品种芒果叶中黄酮的含量研究

用高效液相色谱法测定了13个品种的芒果叶中黄酮的含量。采用HPLC法,色谱柱为C18分析柱(5μm,4.6mm×150 mm);柱温35℃;进样体积为10μL;检测波长360 nm;流速为0.8 m L/min;流动相为甲醇-0.3%磷酸(50︰50)。结果显示,标准品芦丁在12.50~400.00μg/m L范围内与峰面积呈线性关系,相关系数为0.999 7,检出限为0.012μg/m L,平均加样回收率为98.62%(RSD=1.3%)。其中,吉禄芒果叶中黄酮含量最高,其物质含量为0.012 5 mg/kg;黄酮含量最低的是鹰嘴芒,其物质含量为0.007 6 mg/kg。     

Changes in smoking prevalence in Ukraine in 2001-5

Objectives

To analyse trends in smoking prevalence in Ukraine from three surveys conducted in 2001–5, and to explore correlates of observed changes, in order to estimate the stage of tobacco epidemic in Ukraine.

Design

Repeated national interview surveys in Ukraine in 2001, 2002 and 2005.

Main outcome measure

Prevalence of current smoking among the population aged ⩾15 years.

Results

The age‐standardised prevalence of current smoking in Ukrainian men was 54.8% in 2001 and 66.8% in 2005. Among Ukrainian women, prevalence increased from 11.5% in 2001 to 20.0% in 2005. ORs for yearly increase in prevalence were estimated as 1.164 (95% CI 1.111 to 1.220) for men and 1.187 (1.124 to 1.253) for women, which implies that, on average, 3–4% of men and 1.5–2% of women living in Ukraine join the smoking population each year.

Conclusions

In Ukraine, smoking prevalence is increasing in most population groups. Among men, the medium deprivation group with secondary education has the highest smoking prevalence. Among women, while the most educated, young and those living in larger cities are the leading group for tobacco use, other groups are also increasing their tobacco use. Tobacco promotion efforts appear to have been significantly more effective in Ukraine than smoking control efforts. The decrease in real cigarette prices in Ukraine in 2001–5 could be the main factor explaining the recent growth in smoking prevalence.Ukraine is a large eastern European country with high smoking prevalence. Tobacco products are widely available at very low prices, and the transnational tobacco industry is extremely successful in promoting its products and lobbying for its interests in the legislative field. Advocacy of tobacco control has only recently achieved some success in the legislative field, with the first tobacco control law being adopted in late 2005. Ukraine ratified the Framework Convention on Tobacco Control in 2006, but there is still much cause for concern regarding the enforcement and effectiveness of the adopted legislative measures. Unfortunately, the government is not yet involved in nationwide surveillance of the tobacco problem, and the available data have mostly been gathered with funding from foreign donors. Several attempts have been made to measure the extent of the tobacco epidemic in the countries of the former Soviet Union (FSU).^{1,2,3,4,5,6,7} Most of these studies have shown rather high smoking prevalence among men (50–70%) and comparatively low prevalence among women (5–20%). Most countries in the FSU have similar smoking rates, while certain trends are shown to be related to the differences in how the transnational tobacco industry succeeds in every national tobacco market.⁶ Unfortunately, few studies have been published showing trends in smoking prevalence in the FSU.⁷ In Ukraine, two studies^3,4 provided point estimates of smoking prevalence.The aim of this study was to analyse trends in smoking prevalence in Ukraine, on the basis of three surveys conducted in 2001–5, and to explore correlates of observed changes in order to estimate the stage of the tobacco epidemic in Ukraine.     

2010年河南省部分食品中重金属污染状况分析

了解河南省部分食品中重金属污染的现状。方法 在河南省18个省辖市采集8大类3 657份食品样品,按照国家标准检测食品中铅、镉和汞的含量,检测结果按照GB 2762—2012《食品安全国家标准食品中污染物限量》进行评价。结果 河南省部分食品中铅含量的平均值为0.34 mg/kg,总体超标率为8.8%(320/3 656),其中粮食、肉类和蔬菜中超标率较高,分别为17.2%(95/552)、14.5%(85/587)和10.7%(57/534);部分食品中镉含量的平均值为0.054 mg/kg,总体超标率为3.9%(143/3 657),其中食用菌和蛋类中超标率较高,分别为9.6%(49/508)和8.1%(42/518);部分食品中汞含量的平均值为0.077 mg/kg,总体超标率为8.3%(303/3 657),其中蔬菜和粮食中超标率较高,分别为25.3%(135/534)和12.3%(68/551)。结论 河南省部分食品中铅、汞污染情况较为严重,其中粮食、蔬菜和肉类食品中污染情况尤为突出,需要加强监管。     

Moulds and mycotoxins in sorghum stored in traditional containers in India

Various traditional containers have been used in India for storage of sorghum grains. Sorghum is susceptible to fungal infestation and toxin elaboration. The present study relates to the mould and mycotoxin contamination (aflatoxin B₁ and T-2 toxin) in stored sorghum in different storage containers viz. “Kotlu” (Storage rooms), earthenware pots, gunny bags and reed baskets. Aspergillus sp. and Fusarium sp. were the prominent genera and the “Kotlu” form of storage was most susceptible to fungal attack. Storage treatment had little effect on fungal contamination, but despite the fungal infestation, the mycotoxin contamination was found to be very low.     

中国固态发酵白酒中功能细菌研究进展

细菌是白酒酿造3大类微生物之一,其在白酒生产中有着重要的作用,如:芽孢杆菌、乳酸菌、放线菌和梭菌等,它们能产生酯类、有机酸、吡嗪、萜烯等微量成分,从而影响白酒的风味与品质。基于细菌在白酒中的重要功能以及微生物分离培养技术和分析检测技术的进步,近年来相关研究越来越深入。该文综述了近年来白酒功能细菌的研究进展,介绍了酿酒各个环节中主要功能细菌及其在白酒中的作用,旨在为白酒功能细菌的研究提供参考。     

Fungicides in forestry in Great Britain

In Great Britain, fungicides are used in the forest only for the control of root and stem rot, caused by Fames annosus. In forest nurseries they are erriployed on a small scale to control damping-off, grey mould (Botrytis cinerea), needle-cast of pine caused by Lophodermium pinastri, needle-cast of larch caused by Meria laricis, needle blight of Western red cedar (Thuja plicata) caused by Didymascella thujina, and oak mildew (Microsphaera alphitoides).