RP-HPLC测定阿奇霉素缓释阴道栓的含量

目的 建立RP-HPLC测定阿奇霉素缓释阴道栓的含量.方法 用C18(4.6 mm×150 mm,5 μm)柱,以乙腈-磷酸氢二钾溶液(0.02 mol/L)-磷酸二氢钾溶液(0.07 mol/L)溶液(60∶25∶15)为流动相,柱温40℃,流速1.2 mL/min,检测波长215 nm.结果 阿奇霉素的线性范围为60～800 μg/mL,r=0.999 8;低、中、高3种浓度的平均回收率分别为101.4%,99.1%,101.2%.结论 本方法简便、灵敏、准确.     

RP-HPLC测定替比培南酯中聚合物含量

目的建立RP-HPLC测定替比培南酯中聚合物含量的方法。方法采用十八烷基硅烷键合硅胶为填充剂（Waters XBridge C18,5μm,4.6 mm×250 mm）,柱温为40℃;以0.025 mol/L磷酸二氢钠溶液（用1 mol/L氢氧化钠溶液调pH为6.0）-乙腈（50：50）为流动相,流速1.0 mL/min;检测波长220 nm,进样量10μL。结果替比培南酯对照液浓度在5.84～13.63μg/mL范围内具有良好的线性关系（r=0.9992）;对照溶液在24 h内稳定;对照溶液精密度RSD为0.45%;定量限为0.58μg/mL;最低检出限为0.17μg/mL;重复性试验显示本方法重复性良好。结论此法灵敏度高,操作简便,准确可靠,可用于替比培南酯中聚合物含量的测定。     

RP-HPLC法测定薁磺酸钠滴眼液的含量

目的测定薁磺酸钠滴眼液中薁磺酸钠的含量。方法用RP-HPLC法,色谱柱：Dikma C18柱（150 mm×4.6 mm,5μm）;流动相：乙腈-0.02 mol/L磷酸二氢钾水溶液（体积比为33：67,用磷酸调pH 4.5）;检测波长：293 nm;柱温：室温;流速：0.9 mL/min。结果薁磺酸钠在12.0～60.0μg/mL范围内线性关系良好（R=0.999 9）;薁磺酸钠的平均回收率为100.1%,RSD为0.14%。结论该方法简单、快捷,回收率和重复性良好,可作为薁磺酸钠滴眼剂质量评价的方法。     

高效液相色谱法测定痔痛安软膏中苦参碱与氧化苦参碱的含量

目的建立测定痔痛安软膏中苦参碱与氧化苦参碱含量的HPLC方法。方法采用Inertsil C18色谱柱（4.6mm×250 mm,5μm）;以乙腈-0.025 mol/L磷酸二氢钾-0.025 mol/L十二烷基硫酸钠-水（335∶185∶185∶295）为流动相,流速1.0 mL/min,检测波长205 nm。结果苦参碱、氧化苦参碱分别在42～840μg/mL（r=1.000 0,n=6）、9.6～192μg/mL（r=1.000 0,n=6）范围内呈良好的线性关系;平均回收率分别为99.67%（n=6,RSD=1.63%）,98.29%（n=6,RSD=2.11%）。结论该方法简便、灵敏、准确、专属性强,重现性好,可作为痔痛安软膏的质量控制方法。     

高效液相紫外法检测肉鸡组织中的阿奇霉素残留

目的：研究建立反相液相色谱法监控肉鸡组织阿奇霉素的残留。方法：采用C18 柱(4.6mm × 250mm,5μm),乙腈- 异丙醇-0.002mol/L 磷酸氢二钠(60:15:25,V/V)为流动相,紫外检测波长210nm,样品用氯仿- 异丙醇(95:5,V/V)提取,氮气流吹干,加流动相溶解后进样。结果：阿奇霉素在0.05～5.0μg/g 范围内与峰面积呈线性相关,r ＞ 0.990;血清中最低检测限为0.02μg/ml,组织最低定量限为0.05μg/g,血清回收率＞ 83%,组织回收率＞ 77%,RSD ＜ 5%。结论：该方法快速、精确、重复性好,符合肉鸡组织中阿奇霉素残留检测的要求。     

HPLC测定复方妥布霉素滴眼液中苯扎氯铵含量

目的建立HPLC测定复方妥布霉素滴眼液中苯扎氯铵含量的方法。方法以辛烷基硅烷键合硅胶为填充剂;以0.1mol/L乙酸钠溶液(冰乙酸调pH至5.0)-乙腈(40:60)为流动相;检测波长262 nm;流速1.0 mL/min;柱温35℃;进样量20μL。结果苯扎氯铵在0.0645~1.613μg范围内呈良好的线性关系(r=1.000);苯扎氯铵的检测限为8.5 ng,定量限为21.3 ng;苯扎氯铵平均回收率为100.8%(n=9),RSD=1.1%;空白溶液对苯扎氯铵测定无干扰。结论此法准确、可靠,可有效地控制复方妥布霉素滴眼液中苯扎氯铵的含量。     

高效液相色谱法(HPLC)测定山楂片中的熊果酸和齐墩果酸

建立了高效液相色谱同时测定山楂片中熊果酸和齐墩果酸含量的方法。色谱条件：色谱柱Hypersil BDS C18（4.6mm×200mm,5μm）,柱温为25℃,UV检测波长2l0nm,流动相为甲醇-磷酸水溶液（pH=3.0）（85∶15）,流速为0.5mL/min。结果表明：熊果酸和齐墩果酸的线性范围38.0μg/mL～600μg/mL（r=0.9991）和12.5μg/mL～200μg/mL（r=0.9994）,平均回收率分别为99.06%和99.17%,RSD分别为1.43%（n=5）和2.49%（n=5）;该方法简便、准确,适合于山楂片中熊果酸和齐墩果酸含量的测定。     

固相萃取HPLC法同时测定食品中乙基麦芽酚和香兰素

建立了食品中乙基麦芽酚和香兰素的高效液相色谱测定法。方法采用C18（5μm，4．6mm×250mm i．d）反相色谱柱，流动相为乙腈和0．02mol/L磷酸二氢钠溶液，流速1．0mL/min，检测波长276nm，柱温30℃，进样量20μL。该方法的检出限0．5μg/g-2．0μg/g，测定低限饮料1mg/L,-4mg/L，固态食品为5μg/g-20μg/g，线性范围2．0mg／L～100mg/L，加标回收率97．1％～88．7％，相对标准偏差为4．27％～6．74％（n=9）。     

HPLC-MS/MS法检测家禽鸡可食组织中阿奇霉素的残留量

建立了检测家禽鸡可食组织中阿奇霉素残留量的HPLC-MS/MS法,主要色谱条件为:XDB-C18色谱柱(1.8μm,2.1×30mm);以0.1%甲酸的水和甲醇(60∶40,体积比)作为流动相;流量为0.4mL/min;以MRM扫描模式,母离子m/z 749.5,定量离子m/z 589.5,定性离子m/z 157.8进行检测。结果表明:该方法加标线性范围为0.01μg/mL~0.20μg/mL与0.20μg/mL~1.0μg/mL相关系数均大于0.990,出峰时间为1.231 min,最低检测限为0.001μg/mL,采用本法测定鸡可食组织中阿奇霉素回收率在73.6%以上,日内日间变异系数均小于5%。     

酱卤肉制品中食品添加剂的固相提取与精确分析

目的：建立酱卤肉制品中苯甲酸、山梨酸和糖精钠的精确定量方法。方法：样品经乙酸乙酯萃取,SPE-MCX固相萃取处理,采用高效液相色谱（High Performance Liquid Chromatography,HPLC）检测。色谱柱为Agilent ZORBAX Eclipse XDB-C₁₈（250 mm×4.6 mm,5 μm）,流动相为75% 0.02 mol/L乙酸铵水溶液和25%乙腈混合溶液,柱温为25 ℃,流速0.8 mL/min,进样量10 μL;检测波长230 nm。结果：3种添加剂质量浓度在0.5～10.0 mg/L范围内,其峰面积与质量浓度呈良好的线性关系,R²＞0.990,且3种添加剂检测限均低于3.52×10^-2 mg/kg,回收率为95.44%～101.24%,相对标准偏差均小于2.92%。结论：该方法简单、灵敏、快速、准确,适用于酱卤肉制品中苯甲酸、山梨酸和糖精钠3种添加剂的日常检测。     

阿奇霉素和红霉素儿科临床应用的比较

根据临床中遇到的问题,结合相关文献,应用阿奇霉素半衰期计算其在连续用药和间隔用药中每日体内药量,讨论阿奇霉素和红霉素在临床应用中的抗菌作用、半衰期及不良反应。     

138例阿奇霉素致不良反应报告分析

目的 了解阿奇霉素不良反应的临床表现,为临床安全、有效、合理用药提供参考.方法 收集我院2004年1月至2011年2月上报的阿奇霉素不良反应报告138例,并对相关内容分类及分析.结果 阿奇霉素最常见的不良反应为胃肠道反应、注射部位疼痛,此外,有过敏性休克、心血管系统损害等.结论 应进步合理使用阿奇霉素,减少不良反应的发...     

大豆磷脂阿奇霉素脂质体的制备及稳定性研究

利用大豆粉状磷脂,采用逆相蒸发结合冻融法制备阿奇霉素脂质体,以高效液相色谱法为分析手段,采用反透析法测定阿奇霉素脂质体的包封率。研究了阿奇霉素脂质体配方中不同成分的比例,以及水合介质对脂质体包封率的影响。阿奇霉素脂质体的最佳制备条件为：温度38℃,阿奇霉素：磷脂为1：20（质量比）,阿奇霉素：胆固醇为1：2．5（质量比）,最佳的水合介质是pH6．8的磷酸盐缓冲溶液,加入的磷酸盐缓冲溶液为20ml。在此条件下,阿奇霉素脂质体的包封率为72．86％。该方法准确,可用于大豆磷脂阿奇霉素脂质体的制备,并且制备的脂质体稳定。     

138例阿奇霉素致不良反应报告分析

目的了解阿奇霉素不良反应的临床表现,为临床安全、有效、合理用药提供参考。方法收集我院2004年1月至2011年2月上报的阿奇霉素不良反应报告138例,并对相关内容分类及分析。结果阿奇霉素最常见的不良反应为胃肠道反应、注射部位疼痛,此外,有过敏性休克、心血管系统损害等。结论应进一步合理使用阿奇霉素,减少不良反应的发生。     

Reliable identification of grapevine rootstock varieties using RAPD PCR on woody samples

Since grapevine ( Vitis spp .) rootstock material is being traded increasingly as disbudded woody material a lack of distinctive morphological features on such material necessitates an alternative and reliable means of identification. Methods described here were developed for rapid and efficient extraction of DNA from woody samples rich in phenolic compounds and polysaccharides, and for subsequent identification of varieties by RAPD PCR. Using these methods, and with the application of only one selected RAPD primer, we were able to differentiate sixteen rootstock varieties, including the seven varieties most commonly used in Germany. Problems commonly encountered with reproducibility of RAPD patterns were avoided by choosing primers with a dinucleotide sequence and a high G/C content that allowed a rather high annealing temperature of 45°C. Methods described here should also be useful for other horticultural crops, especially those with woody tissues rich in phenolic compounds and polysaccharides.     

An internet compendium of analytical methods and spectroscopic information for monomers and additives used in food packaging plastics

An internet website (http://cpf.jrc.it/smt/) has been produced as a means of dissemination of methods of analysis and supporting spectroscopic information on monomers and additives used for food contact materials (principally packaging). The site which is aimed primarily at assisting food control laboratories in the European Union contains analytical information on monomers, starting substances and additives used in the manufacture of plastics materials. A searchable index is provided giving PM and CAS numbers for each of 255 substances. For each substance a data sheet gives regulatory information, chemical structures, physico-chemical information and background information on the use of the substance in particular plastics, and the food packaging applications. For monomers and starting substances (155 compounds) the infra-red and mass spectra are provided, and for additives (100 compounds); additionally proton NMR are available for about 50% of the entries. Where analytical methods have been developed for determining these substances as residual amounts in plastics or as trace amounts in food simulants these methods are also on the website. All information is provided in portable document file (PDF) format which means that high quality copies can be readily printed, using freely available Adobe Acrobat Reader software. The website will in future be maintained and up-dated by the European Commission's Joint Research Centre (JRC) as new substances are authorized for use by the European Commission (DG-ENTR formerly DGIII). Where analytical laboratories (food control or other) require reference substances these can be obtained free-ofcharge from a reference collection housed at the JRC and maintained in conjunction with this website compendium.     

Aroma characterization of various apricot varieties using headspace–solid phase microextraction combined with gas chromatography–mass spectrometry and gas chromatography–olfactometry

The characterization of the aromatic profile of several apricot cultivars with molecular tracers in order to obtain objective data concerning the aromatic quality of this fruit was undertaken using headspace–solid phase microextraction (HS–SPME). Six apricot cultivars were selected according to their organoleptic characteristics: Iranien, Orangered, Goldrich, Hargrand, Rouge du Roussillon and A4025. The aromatic intensity of these varieties measured by HS–SPME–Olfactometry were defined and classified according to the presence and the intensity of grassy, fruity and apricot like notes. In the six varieties, 23 common volatile compounds were identified by HS–SPME–GC–MS. Finally, 10 compounds, ethyl acetate, hexyl acetate, limonene, β-cyclocitral, γ-decalactone, 6-methyl-5-hepten-2-one, linalool, β-ionone, menthone and (E)-hexen-2-al were recognized by HS–SPME–GC–O as responsible of the aromatic notes involved in apricot aroma and considered as molecular tracers of apricot aromatic quality which could be utilized to discriminate apricot varieties.     

Tests of potential functional barriers for laminated multilayer food packages. Part I: Low molecular weight permeants

The advent of the functional barrier concept in food packaging has brought with it a requirement for fast tests of permeation through potential barrier materials. In such tests it would be convenient for both foodstuffs and materials below the functional barrier (sub-barrier materials) to be represented by standard simulants. By means of inverse gas chromatography, liquid paraffin spiked with appropriate permeants was considered as a potential simulant of sub-barrier materials based on polypropylene (PP) or similar polyolefins. Experiments were performed to characterize the kinetics of the permeation of low molecular weight model permeants (octene, toluene and isopropanol) from liquid paraffin, through a surrogate potential functional barrier (25 μm-thick oriented PP) into the food simulants olive oil and 3% (w/v) acetic acid. These permeation results were interpreted in terms of three permeation kinetic models regarding the solubility of a particular model permeant in the post-barrier medium (i.e. the food simulant). The results obtained justify the development and evaluation of liquid sub-barrier simulants that would allow flexible yet rigorous testing of new laminated multilayer packaging materials.