盐析法提取聚季铵盐-7中残余丙烯酰胺的研究

采用硫酸钠将聚季铵盐-7高聚物析出,然后用甲醇／异丙醇对其中的残留单体丙烯酰胺（AM）进行提取,同时用高效液相色谱对提取液中的丙烯酰胺进行测定,得到了最佳提取方案：V（甲醇）：V（异丙醇）：1：1,搅拌提取时间60min;最佳色谱条件为：流动相V（甲醇）：V（水）=4：96,流速1．0mL／min;在最佳条件下测试回收率在97．37％～99．68％范围内,相对标准偏差为2．96％。     

HPLC测定润滑油中的NMP

建立了一种分析NMP的高效液相色谱方法,色谱条件：色谱柱为VARIAN C18（250×4．6nm）,流动相为m（甲醇）：m（水）=40：60,流速1mL／min,柱温为室温,检测波长210nm。方法线性范围为0．0001％-0．01％,r=0．9996,检出限为0．002μg,RSD为0．10％,加标回收率为98．6％-100．7％。能够快速、精确测定润滑油精制工艺过程中NMP的含量。     

吡螨胺的反相高效液相色谱分析

建立了一种用高效液相色谱测定吡螨胺的定量分析方法,采用C18HPLC色谱柱,以V（甲醇）：V（水）=90：10为流动相。选择200nm为检测波长进行检测,结果表明本方法的标准偏差为0．0014,变异系数为0．1581％,相关系数为0．99991,平均回收率为99．78％。     

RP-HPLC法测定落叶松中二氢槲皮素的含量

采用反相高效液相色谱法测定落叶松中二氢槲皮素的含量。确定色谱条件为：色谱柱Hypersil ODS—C18（4．6mm×200mm,5μm）;流动相为V（甲酵）：V（水）：V（冰醋酸）=40：59：1;流速为1．0mL·min^-1;检测波长为288nm;柱温为28℃。在此条件下,二氢槲皮素与其它组分得到良好的分离。线性范围为0．02～0．2μg·μL^-1（r=0．9998）,精密度RSD为0．96％（n=5）,平均回收率为100．4％。     

2-肼基-4,6-二甲基嘧啶的高效液相色谱分析

用高效液相色谱外标法对2-肼基-4,6-二甲基嘧啶进行定量分析,以V甲醇：V水=90：10为流动相,采用Kromasil 100-5C18色谱柱和紫外检测器。方法标准偏差为0．053,变异系数为0．024％,平均回收率为99．6％。     

4，4′-二（羟甲基）联苯合成回收溶剂中二甲亚砜含量的测定方法

采用高效液相色谱法测定4,4′-二（羟甲基）联苯合成后回收溶剂中二甲亚砜的含量。方法采用Zorbax SB-C18色谱柱,以甲醇-水（v：v=13：7）为流动相,检测波长为210nm,标准曲线外标法测定回收溶剂中二甲亚砜的含量。二甲亚砜在0．08-0．58mg／mL浓度范围内与峰面积呈线性关系,回归方程：y=14．8594x＋154．7371,相关系数r=0．99996。平均回收率为100．59％,RSD为0．69％（n=6）。     

反相高效液相色谱法测定化妆品中的3—O-乙基维生素C

采用反相高效液相色谱法测定化妆品中的3—O-乙基维生素C,色谱条件：SHIMADZU Shim-pack VP-C18ODS（150mm×4．6mm,5μm）色谱柱;C18ODS保护柱芯;流动相V（甲醇）：V（0．025mol/L KH2PO4）=20：80;流速：1．0mL/min;柱温：30℃;紫外检测器检测,检测池温度：40℃,波长：254nm。结果表明,在此条件下,3—O-乙基维生素C在0-100mg／L与相应的峰面积具有良好的线性关系（r=0．9992）,线性回归方程为A=31．1703ρ,回收率在97．75％-100．60％,方法精密度RSD约为2．6％（n=5）。     

2，4-滴丁酯·磺草酮乳油的高效液相色谱分析

采用高效液相色谱法,以Century C18（200×4．6mm,5μm）为固定相,以乙腈＋水（磷酸调pH值为2．5）=700＋300（V＋V）为流动相,流速1．0mL·min^-1,检测波长235nm,在同一色谱条件下同时测定2,4-滴丁酯·磺草酮乳油中的2,4-滴丁酯和磺草酮。2,4-滴丁酷变异系数为0．46％,平均回收率为99．88％,磺草酮变异系数为0．58％,平均回收率为99．92％。     

2，4-滴丁酯·扑草净·异丙草胺乳油的高效液相色谱分析

采用高效液相色谱法,以KromasilC-18（200X4．6mm,5μm）为固定相,以四氢呋喃＋水（磷酸调pH：3．3）=500＋500（V＋y）为流动相,流速1．0mL·min-1,检测波长270nm,柱温40℃,在同一色谱条件下同时测定2,4-滴丁酯·扑草净·异丙草胺乳油中的2,4-滴丁酯、扑草净和异丙草胺。2,4-滴丁酯变异系数为0．62％,平均回收率为99．64％;扑草净变异系数为0．68％,平均回收率为99．81％;异丙草胺变异系数为0．48％,平均回收率为100．04％。     

柱前衍生反相高效液相色谱法快速测定3,5-二氯苯甲酰氯

以无水甲醇作柱前衍生试剂，建立了反相高效液相色谱法间接测定3，5-二氯苯甲酰氯的新方法。实验结果表明，在流动相：甲醇-水（85：15），流速：1．0mL／min，检测波长：288nm的条件下，定量校正曲线具有良好的线性关系，相关系数（r）为0．9999。方法用于样品中标题物质的测定，RSD=0．19％（n=6），加标回收率为99．9％-105％。     

制备型高效液相色谱法分离冬凌草中冬凌草甲素

采用反相高效液相色谱技术,分离制备冬凌草中冬凌草甲素。制备色谱条件:色谱柱(80 mm i.d×500mm,μBondapakTMC18,粒径25~40μm);柱温:40℃;流动相:V(CH3OH)∶V(H2O)=50∶50;流速60 mL/min;检测波长239 nm;进样体积10 mL。将所收集16~23 min的洗脱液经蒸发浓缩,真空干燥,得冬凌草甲素白色粉末。160 g冬凌草可提取出500 mg冬凌草甲素(质量分数>99.0%)。采用质谱、元素分析、紫外、红外、核磁共振氢谱和高效液相色谱方法,鉴定和验证了提取物的结构。     

复配农药制剂阿维菌素·哒螨灵的高效液相色谱分析

采用反相高效液相色谱法同时测定阿维菌素与哒螨灵的复配农药制剂。实验表明,在波长254 nm,流动相CH3CN∶CH3OH∶H2O=40∶40∶20(体积比),流速1.5 mL/min的条件下,其线性相关系数分别为0.998 8和0.999 3,相对标准偏差为0.58和3.72,平均回收率为99.50和99.32。     

Antibacterial Activity of Hexadecynoic Acid Isomers toward Clinical Isolates of Multidrug-Resistant Staphylococcus aureus

In the present study, the structural characteristics that impart antibacterial activity to C₁₆ alkynoic fatty acids (aFA) were further investigated. The syntheses of hexadecynoic acids (HDA) containing triple bonds at C-3, C-6, C-8, C-9, C-10, and C-12 were carried out in four steps and with an overall yield of 34–78%. In addition, HDA analogs containing a sulfur atom at either C-4 or C-5 were also prepared in 69–77% overall yields, respectively. Results from this study revealed that the triple bond at C-2 is pivotal for the antibacterial activity displayed by 2-HDA, while the farther the position of the triple bond from the carbonyl group, the lower its bactericidal activity against gram-positive bacteria, including clinical isolates of methicillin-resistant Staphylococcus aureus (CIMRSA) strains. The potential of 2-HDA as an antibacterial agent was also assessed in five CIMRSA strains that were resistant to Ciprofloxacin (Cipro) demonstrating that 2-HDA was the most effective treatment in inhibiting their growth when compared with either Cipro alone or equimolar combinations of Cipro and 2-HDA. Moreover, it was proved that the inhibition of S. aureus DNA gyrase can be linked to the antibacterial activity displayed by 2-HDA. Finally, it was determined that the ability of HDA analogs to form micelles can be linked to their decreased activity against gram-positive bacteria, since critical micellar concentrations (CMC) between 50 and 300 μg/mL were obtained.     

抗氧剂2088的HPLC分析方法

研究了用HPLC分析抗氧剂2088（2，4-二（正辛硫基亚甲基）-6-甲基苯酚）含量的方法。采用Agilent1100型高效液相色谱仪、EclipseXDB—C18色谱柱，以甲醇和水混合溶剂（体积比90：10）做流动相，流速为0．4mL／min，紫外检测波长为285啪的条件时，样品中的各组分达到较好的分离，以峰面积对浓度做标准曲线，线性回归方程为Y=137．2X-26．227，相关系数为r=0．9852。     

Beyond 9-ODA: SEX Pheromone Communication in the European Honey Bee Apis mellifera L.

The major component of the mandibular gland secretion of queen honeybees (Apis mellifera L.), 9-ODA ((2E)-9-oxodecenoic acid), has been known for more than 40 yr to function as a long-range sex pheromone, attracting drones at congregation areas and drone flyways. Tests of other mandibular gland components failed to demonstrate attraction. It remained unclear whether these components served any function in mating behavior. We performed dual-choice experiments, using a rotating drone carousel, to test the attractiveness of 9-ODA compared to mixtures of 9-ODA with three other most abundant components in virgin queen mandibular gland secretions: (2E)-9-hydroxydecenoic acid (9-HDA), (2E)-10-hydroxydecenoic acid (10-HDA), and p-hydroxybenzoate (HOB). We found no differences in the number of drones attracted to 9-ODA or the respective mixtures over a distance. However, adding 9-HDA and 10-HDA, or 9-HDA, 10-HDA, and HOB to 9-ODA increased the number of drones making contact with the baited dummy. On the basis of these results, we suggest that at least 9-HDA and 10-HDA are additional components of the sex pheromone blend of A. mellifera.     

Drones of the Dwarf Honey Bee <Emphasis Type="Italic">Apis Florea</Emphasis> Are Attracted to (2E)-9-Oxodecenoic Acid and (2E)-10-Hydroxydecenoic Acid

The queen mandibular gland component (2E)-9-oxodecenoic acid (9-ODA) has been suggested to function as the major sex pheromone component in all honey bee species. In contrast to this hypothesis, chemical analyses showed that in the Asian dwarf honey bee species, Apis florea, a different decenoic acid, (2E)-10-hydroxydecenoic acid (10-HDA), is the major component in the mandibular gland secretion. We show here that A. florea drones are attracted to 9-ODA as well as to 10-HDA. However, 10-HDA attracted higher numbers of drones at lower dosages than 9-ODA, and also was more attractive when directly compared to 9-ODA in a dual attraction experiment. We conclude that 10-HDA has to be viewed as the major sex pheromone in A. florea. The result that both pheromone components are capable of attracting drones when presented alone was unexpected with regard to existing sex pheromone attraction experiments in honey bees.     

高效液相色谱法测定Famoxadone在苹果中的残留量研究

建立了测定易保(Equationcontact)中有效成分Famoxadone在苹果中残留量的高效液相色谱分析方法。色谱柱选择Novapak苯基柱3.9mm×150mm(填充物粒径4μm);流动相为乙腈+0.01mol/L磷酸二氢钾(体积比为45:55,pH=3);固定柱温40℃。测定的回收率均在82%以上,相对标准偏差小于5.58%,最低检测限为2×10-9g。     

Rapid Detection and Quantification of Triacylglycerol by HPLC–ELSD in Chlamydomonas reinhardtii and Chlorella Strains

Triacylglycerol (TAG) analysis and quantification are commonly performed by first obtaining a purified TAG fraction from a total neutral lipid extract using thin-layer chromatography (TLC), and then analyzing the fatty acid composition of the purified TAG fraction by gas chromatography (GC). This process is time-consuming, labor intensive and is not suitable for analysis of small sample sizes or large numbers. A rapid and efficient method for monitoring oil accumulation in algae using high performance liquid chromatography for separation of all lipid classes combined with detection by evaporative light scattering (HPLC–ELSD) was developed and compared to the conventional TLC/GC method. TAG accumulation in two Chlamydomonas reinhardtii (21 gr and CC503) and three Chlorella strains (UTEX 1230, CS01 and UTEX 2229) grown under conditions of nitrogen depletion was measured. The TAG levels were found to be 3–6 % DW (Chlamydomonas strains) and 7–12 % DW (Chlorella strains) respectively by both HPLC–ELSD and TLC/GC methods. HPLC–ELSD resolved the major lipid classes such as carotenoids, TAG, diacylglycerol (DAG), free fatty acids, phospholipids, and galactolipids in a 15-min run. Quantitation of TAG content was based on comparison to calibration curves of trihexadecanoin (16:0 TAG) and trioctadecadienoin (18:2 TAG) and showed linearity from 0.2 to 10 μg. Algal TAG levels >0.5 μg/g DW were detectable by this method. Furthermore TAG content in Chlorella kessleri UTEX 2229 could be detected. TAG as well as DAG and TAG content were estimated at 1.6 % DW by HPLC–ELSD, while it was undetectable by TLC/GC method.     

HBIW的纯度分析方法

研究了流动相、流速、柱温等因素对HBIW纯度分析的影响.建立了HBIW的高效液相色谱分析条件:反相色谱柱,紫外检测波长241nm,二元流动相四氢呋喃-水体积比90:10,流速1.000mL/min,柱温25℃.采用归一化法、外标法和内标法对HBIW进行了纯度分析.结果表明,3种方法标准偏差均小于1%,归一化法准确度受样...     

反相高效液相色谱法同时测定乳酸及乳酸甲酯

乳酸及乳酸甲酯是重要的有机化工原料。在由乳酸合成乳酸甲酯的绿色化工工艺研究过程中,为了优化反应条件,建立了一种同时分离测定乳酸连续酯化反应体系中乳酸和乳酸甲酯的反相高效液相色谱法。HPLC分析条件为:Prevail C18色谱柱,以V〔NaH2PO4/H3PO4缓冲液(pH2.0)〕:V(甲醇)=90∶10为流动相,流速为1.0 mL.m in-1,检测器为示差折光检测器。在进样量为0.2~20μg成良好的线性关系。乳酸的加样回收率为94.55%~106.94%,相对标准偏差为1.23%~2.01%;乳酸甲酯的加样回收率为91.03%~109.0%,相对标准偏差为1.25%~2.88%。该方法准确、简捷、可靠。