Fingerprint Features of Different Varieties of FLOS CHRYSANTHEMI

[Objective] To compare the fingerprint features of different varieties of FLOS CHRYSANTHEMI,and to lay foundation for the establishment of HPLC fingerprint chromatogram of FLOS CHRYSANTHEMI. [Methods] HPLC fingerprint chromatograms of different varieties of FLOS CHRYSANTHEMI were analyzed,which were collected from Tongxiang Germplasm Resources Garden in Zhejiang Province. The correlations of different varieties of FLOS CHRYSANTHEMI were researched by similarity analysis,cluster analysis and principal component analysis. [Results] HPLC fingerprint chromatograms of FLOS CHRYSANTHEMI were established,showing that there was certain similarity in HPLC chromatograms of different varieties. A total of 13 common peaks were screened. Results of fingerprint data,cluster analysis and principal component analysis showed the connection of different varieties of FLOS CHRYSANTHEMI in regionality and genetic relationship,as well as their unique characteristics. [Conclusions]The chromatographic system could be used for establishing the fingerprints of different varieties of FLOS CHRYSANTHEMI,which provided references for the application,quality evaluation and germplasm selection of FLOS CHRYSANTHEMI.     

Problems and Countermeasures for Industrialized Cultivation of FLOS CHRYSANTHEMI Grown in Tongxiang City of China

Cultivation and management status of FLOS CHRYSANTHEMI grown in Hangzhou(Hangzhou FLOS CHRYSANTHEMI) were investigated in Shimen Town of Tongxiang City in the year 2014. Unreasonable fertilization was found in industrialized cultivation of Hangzhou FLOS CHRYSANTHEMI,as well as single cultivation mode,inadequate utilization of straws and so on. Finally,several suggestions were put forward for the planting of Hangzhou FLOS CHRYSANTHEMI in Tongxiang City.     

Content Determination of Total Flavonoids in Food Products of Fagopyrm tataricum(Linn) Gaench

[Objective] To detect the total flavonoids content in food products of Fagopyrm tataricum(Linn) Gaench by UV spectrophotometry.[Methods] Reflux method was used for extraction. Absorbance value was detected by Na NO2- Al(NO3)3method; and the total flavonoids content was calculated with rutin as the reference. [Results] Rutin concentration had good linear relationship with absorbance value when the concentration range was 0. 003- 0. 161 mg / m L,with R2= 0. 995 9. The average recovery rate was 98. 305% and RSD was 1. 62%.[Conclusions]There were significant differences in the total flavonoids contents in twenty F. tataricum foods; their contents were in the order of buckwheat breakfast cereal(3. 813 mg / g) buckwheat rice(3. 115 mg / g) buckwheat noodle(0. 178- 2. 186 mg / g) buckwheat sachima(0. 228- 0. 573 mg / g) buckwheat biscuit(0. 015- 0. 065 mg / g). This method was rapid,simple,accurate and repeatable,and could be used for the content detection of total flavonoids in F. tataricum foods.     

一种同时测定鱼腥草中百草枯和乙草胺残留方法探讨

采用高速匀浆提取,固相萃取(SPE)净化,三重四级杆气相色谱质谱联用仪(GC-MS/MS)检测,建立了鱼腥草中两种除草剂农药残留的分析方法。在0.02~0.50 mg/L范围内,目标物的峰面积与其质量浓度的线性关系良好(R20.99);在0.02、0.10、0.50 mg/kg的添加水平,样品添加回收率为73.5%~81.2%,相对标准偏差(RSD)为3.43%~4.49%;乙草胺方法检出限为0.2μg/kg,定量限为0.80μg/kg,百草枯方法检出限为1.40μg/kg,定量限为5.00μg/kg。该方法具有高灵敏度、快速、准确度高、线性范围宽等优点,可满足鱼腥草中农药残留检测的要求。     

食用菌中SO_2残留快速测定方法的研究

对食用菌中SO2残留的快速测定方法及各种影响因素进行了研究。样品经酸化后,用预经痕量碘蒸气致蓝色的淀粉指示纸检测,样品产生的SO2使其褪色。淀粉指示纸的制备方法、观察时间和测定温度均对检测结果有影响。该测定法对SO2的最小检测限为5mg/L,可用于食用菌产品中SO2残留量的定性检测和半定量分析,具有快速和简便的特点。     

大体积进样离子色谱法测定饮用水中溴酸盐等7种无机阴离子

建立大体积进样,离子色谱法(IC)测定饮用水中不同数量级F-,BrO3-,Cl-,Br-,NO2-,NO3-,SO4-等7种无机阴离子的新方法。采用离子色谱碳酸盐等度淋洗系统,高容量色谱分析柱AS-23,DS5电导检测器,500μL定量环直接进样分析饮用水中7种无机阴离子的保留时间等,并通过峰面积法定量各种阴离子含量。该法各离子线性相关性好(R>0.999 0),精密度高(RSD<3.6%),准确度好(平均回收率96.5%～102.4%),检出限低(3.56～6.74μg/L,以500μL进样量计算)。可同时测定饮用水中不同数量级浓度的7种无机阴离子,检出限低,操作简便,快速准确,不仅能够满足水质监测要求,而且大幅提高检测效率。     

X射线荧光光谱法快速检测原料公干鱼中的镉

旨在建立一种基于X射线荧光光谱法快速检测原料公干鱼(原料鱼)中镉的方法。应用X射线荧光光谱法快速检测原料鱼初始样及干燥样中的镉含量,对快速检测与标准检测结果的相关性进行了分析;考察了对原料鱼进行快速干燥处理的可行性;采用原料鱼的标准测定值对X射线荧光光谱仪进行校正后,考察了快速检测方法的精密度、检测限、准确度等性能参数。结果表明:X射线荧光光谱法能准确测定原料鱼干燥样中的镉,检测限达0.088 mg/kg,线性范围为0.088~1.286 mg/kg,相对标准偏差低于10%。该快速检测方法测定单个样品只需40 min左右,可满足现场对原料鱼中镉的快速测定要求,为防控原料鱼食品中镉超标风险提供了一种高效的筛查手段。     

亲水性液相色谱串联质谱法测定红甜菜中甜菜碱含量

为了建立红甜菜中甜菜碱的定量分析方法,采用改进的QuEChERS方法结合液相色谱串联质谱技术,样品经快速溶剂萃取仪以甲醇为溶剂提取,经固相萃取柱净化,采用正向亲水性液相色谱柱(Hilic),梯度洗脱,通过质谱的多反应监测(multiple reactions monitoring,MRM)正离子模式扫描进行测定,外标法定量。结果表明：甜菜碱在本方法的线性范围为0.05~5 ug/mL,添加水平为4~16 mg/g时,回收率为87.7%~95.7%,方法RSD值为3.69%~8.4%,检出限为0.01 mg/L,定量限为0.04 mg/L,与传统的分析方法相比,具有检出限低、灵敏度高的优点,完全可以适用于甜菜中甜菜碱的分析。     

QuEChERS-高效液相色谱-串联质谱法测定水稻中氯虫苯甲酰胺和噻虫胺的残留

为了监测水稻中氯虫苯甲酰胺和噻虫胺的残留量，本文建立了分散固相萃取的QuEChERS法结合超高效液相色谱串联质(UPLC-MS/MS)同时测定糙米、稻壳、秸秆中氯虫苯甲酰胺和噻虫胺残留量的测定方法。样品经乙腈水振荡提取，PSA或C₁₈净化，UPLC-MS/MS多反应离子监测模式(MRM)下检测，外标法定量。结果表明：氯虫苯甲酰胺和噻虫胺最佳提取溶剂为50%乙腈水，提取方式为振荡提取，选择C₁₈作为糙米提取液的净化剂，PSA作为稻壳和秸秆提取溶剂的净化剂。氯虫苯甲酰胺在0.1~100 μg/L、噻虫胺胺在0.1~500 μg/L范围内线性关系良好，相关系数R²均大于0.99；两种农药在糙米、稻壳和秸秆中的平均添加回收率在83.2%~105.4%之间，相对标准偏差为1.2%~10.1%；氯虫苯甲酰胺和噻虫胺在糙米中定量限为0.005 mg/kg，在稻壳和秸秆中均为0.025 mg/kg。该方法前处理过程操作简单快速，灵敏度高，适用于同时检测糙米、稻壳、秸秆中氯虫苯甲酰胺和噻虫胺的残留量。     

高效液相色谱法测定牛奶中双乙酸钠

建立了牛奶中双乙酸钠的快速测定方法,为执法提供技术支持。牛奶样品用水提取,加入硫酸锌溶液(0.5 mol/L)和氢氧化钾溶液(0.5 mol/L)沉淀、超声、离心,用C18柱分离,二极管阵列检测器测定,外标法定量。色谱条件:Agilent TC-C18色谱柱,流动相为质量浓度1.5 g/L磷酸氢二铵溶液与甲醇体积比为90:10,流速1mL/min。线性范围10～500μg/mL,相关系数R~2=0.99957,定量检测限50 mg/kg,空白样品添加50,100,500μg/mL 3个水平,回收率为101.12%～103.68%,相对标准偏差为2.01%～3.93%(n=6),说明方法准确可靠。     

果蔬中单宁测定技术研究

为研究、建立快速、简便测定蔬菜、水果中单宁含量的方法,选用当前测定单宁应用最为广泛的可见分光光度法为基础进行可行性研究。采用配对t检验,用同一样品对不同单宁提取溶剂、温度和时间及测定的显色时间分别进行比较测定,从而选出最佳单宁提取和测定条件,并对建立的方法进行线性、精密度、准确度等的验证试验。确定了最佳的提取和检测条件为500W超声波提取,超声时间20min,提取溶剂水,温度60℃,显色时间1h。单宁测定线性范围为0~30mg/L,方法检出限0.2mg/g,加标回收率为95.8%~101.9%,相对标准偏差(RSD)1.07%~4.29%。该法具有操作简便、快速、精密度高、重现性好、加标回收率较高、分析成本低等特点。适合于果蔬中单宁酸的快速检测。     

Content Detection of Total Flavonoids in Melastom adodecandnun Lour.

[Objective] To establish a content detection method for the total flavonoids in Melastom adodecandnun Lour. [Methods]Content of total flavonoids in M. adodecandnun was detected by UV-Vis spectrophotometry. [Results]When the content of total flavonoids in M. adodecandnun was detected by UV-Vis spectrophotometry,there was good linear relationship(r = 0. 999 6) within the range of 0. 004 16- 0. 066 59mg/mL. The average recovery rate was 98. 85% and RSD was 2. 75%. [Conclusions]This method was accurate,simple and could be used for the content detection of total flavonoids in M. adodecandnun.     

改良QuEChERS方法结合气相色谱测定红甜菜中20种农药残留

建立了改良的QuEChERS法结合气相色谱-电子捕获检测器用于红甜菜中20种农药残留的联合测定方法。样品中农药残留以乙腈作为提取溶剂,多壁碳纳米管分散固相萃取去除杂质,过滤后经RTX-1色谱柱分离,GC-ECD检测,外标法定量。探讨了气相色谱的程序升温条件,考察了不同提取溶剂及不同的净化方法对检测结果的影响。结果表明：在优化的色谱条件下,20种农药在0.01~0.50 mg/L（莠去津为0.03~0.50 mg/L）范围内线性关系良好,相关系数(R²)均大于0.99,并且得到很好的分离;乙腈与样品的比例为1:2,多壁碳纳米管用量为10 mg的前处理条件下,红甜菜样品在3个浓度的平均回收率为62.0%~116.5%之间,相对标准偏差为1.9%~10.9%,检出限为0.12 µg/L~0.063 mg/L,定量限为0.4 µg/L~0.21 mg/L。该方法操作简单、快速、准确,适用于红甜菜中有机氯及拟除虫菊酯类多农药残留的检测。     

Study on Hybridation and Aseptic Seeding as Well as Rapid Propogation of Demdrobium officinale and Dendrobium aduncum

[Objective]To study the system of aseptic seeding and rapid propogationtin of hybrid seeds of Demdrobium officinale and Dendrobium aduncum [Methods] Demdrobium officinale and Dendrobium aduncum were the objects of research,and their hybrid seeds were gained by artificially auxiliary hybridation. The seeds were induced to germinate in vitro,and study on the technology of aseptic seeding was finished. [Results]Successful hybridation of Demdrobium officinale and Dendrobium aduncum could be easily realized,and hybrid fruit-bearing rate could reach 80%; the suitable culture medium for seeds was: MS +1. 0 mg/L 6-BA +0. 1 mg/L NAA,the germination rate after 30 d of cultivation was 89. 7%; appropriate culture medium for proliferation of protocorm was: MS + 1. 5 mg /L 6-BA + 0. 1 mg /L NAA + 100 g /L banana + 1. 0 mg /L AC; appropriate culture medium for differentiation of protocorm was: MS + 1. 5 mg /L 6-BA + 0. 1 mg /L NAA + 200 g /L potato + 1. 0 g /L AC; the formula of culture medium for strenghening the seedlinge and nurturing the rooting was: 1 /2 MS + 0. 6 mg /L NAA +100 g /L banana + 1. 0 g /L AC,the plant grew robustly,the rooting percentage was 100%,and the survival rate of transplanting was higher than 95%. [Conclusions]This method ascertains the optimum culture media formula in the whole regeneration process and all phases from seed germination to acclimatization and transplantation,so fine solidation is laid for its germplasm innovation and industrialized seedling production.     

超声提取—气相色谱法测定油脂中胆固醇

建立了毛细管气相色谱法测定油脂中胆固醇含量的方法,改进了油脂皂化方法以及皂化完成后使用分液漏斗提取胆固醇过程中容易产生乳化、操作复杂且比较耗时的缺点,采用超声波提取胆固醇,优化了样品前处理条件.结果表明,该法在0.002mg/mL～0.500mg/mL范围呈线性(r=0.9997),检出限为20mg/kg,RSD=1.104％,回收率在81.3％～93.8％之间.     

Extraction Technology and Anti-depression Activity of Saponins from Lilium brownii

[Objective]To investigate the extraction technology of saponins from lily(Lilium brownii) and the anti-depressant activity of saponins. [Methods]The saponins extraction was optimized by an L9(34) orthogonal design with the volume fraction of ethanol,amount of ethanol,extraction time as factors,using saponins extraction rate as index. Kunming mice tested were divided into normal control group(constant volume of normal saline),fluoxetine group(0. 004 g /kg) and high-dose,medium-dose and low-dose lily saponins groups(0. 1,0. 05 and0. 025 g /kg). The duration of immobility within 4 min were recorded in tail suspension test and forced swimming test. Body temperatures of mice were recorded at 4 h after modeling in reserpine-induced hypothermia test. [Results]The optimal extraction technology of lily saponins was as follows: extraction with 70% ethanol once,lasting for 3 h. Compared with normal control group,the duration of immobility within 4 min in tail suspension test and forced swimming test were decreased in medium-dose and low-dose lily saponins groups(P 0. 05); the body temperature of mice was decreased at 4 h after modeling(P 0. 05). [Conclusions]Lily saponins have certain anti-depressant activity in mice.     

双氟磺草胺在土壤中的残留分析

[目的]建立双氟磺草胺在土壤中的残留分析方法。[方法]土壤样品经乙腈振荡提取,静置后过膜,HPLC-PAD直接测定。[结果]当添加质量分数为1.0和10.0 mg/kg时,双氟磺草胺在黄壤、水稻土和石灰土中的添加平均回收率分别为82.4%～86.6%、83.0%～87.7%和85.6%～85.9%,RSD分别为1.9%～2.3%、0.6%～8.2%和2.3%～3.4%。方法最小检出量为1.0×10-9g,土壤中最小检出浓度为1.0 mg/kg。[结论]该方法操作简单,样品分析速度快,准确度、精密度及灵敏度均满足农药残留分析的要求,可用于土壤中双氟磺草胺残留量的检测。     

平菇和榆黄蘑及培养料中的三唑酮的残留动态研究

为制定三唑酮在食用菌上的残留安全标准,在吉林农业大学食用菌基地进行栽培培养,采用子实体喷药、培养料拌药的方法进行残留动态试验,通过气相色谱-质谱联用仪测定分析三唑酮在子实体和培养料中的残留量和残留动态。结果表明,三唑酮在食用菌及培养料中的降解过程均符合一级动力学方程,三唑酮在食用菌和培养料的半衰期分别为2.3~3.1天和14.2天。平菇、榆黄蘑及其培养料在收获时期的三唑酮残留量均小于0.01 mg/kg。证明试验建立的检测方法准确可靠,并为在食用菌上制定的MRL值提供了科学依据。     

超高效液相色谱法测定发芽糙米中γ-氨基丁酸含量

为发芽糙米中γ-氨基丁酸的含量检测提供高效的方法,采用超高效液相色谱柱Waters BEH C₁₈(1.7 μm, 100 mm×2.1 mm),以60%的乙醇为提取剂,流动相组成为乙腈和纯水,以邻苯二甲醛为衍生剂提对γ-氨基丁酸含量进行测定。该方法确定了样品最佳衍生反应时间为2 min,衍生物可在室温条件下稳定时间24 h以上或4℃低温保存。在此条件下绘制了γ-氨基丁酸的标准曲线,线性关系良好,检出限为0.5 mg/L,回收率范围98.88%~99.2%,相对标准偏差为0.6%~2.2%。该方法准确、灵敏、省时,为发芽糙米中γ-氨基丁酸的含量测定奠定了有效可靠的方法基础,可广泛应用。     

利用HPLC-ICP-MS方法测定中华绒螯蟹不同形态砷的残留量

采用高效液相色谱串联电感耦合等离子体质谱仪(HPLC-ICP-MS)测定中华绒螯蟹可食部位6种砷形态的残留量。经过前处理、提取和脱脂后,通过色谱柱、流动相、pH和流速等参数调节,筛选得到最优化的分离和检测条件。结果表明,6种砷形态的混合标准溶液在质量浓度0~50 μg/L范围时,均呈现良好的线性关系,其R²达到0.999,检测限为0.0060~0.0912 μg/kg,定量限为0.020~0.304 μg/kg。在样品中添加0.5、5、50 μg/L浓度水平,回收率良好,范围是70%~120%,相对标准偏差(RSD)均<5%,方法精密度与重复性均良好。本方法为中华绒螯蟹可食部位砷形态残留量建立了有效检测方法,为水产品砷残留快速检测提供技术支撑。