Biodegradation of Gaseous Chlorobenzene by White-rot Fungus Phanerochaete chrysosporium

Objective To evaluate the effect of white rot fungus Phanerochaete chrysosporium on removal of gaseous chlorobenzene. Methods Fungal mycelium mixed with a liquid medium was placed into airtight bottles. A certain amount of chlorobenzene was injected into the headspace of the bottles under different conditions. At a certain interval, the concentrations in the headspace were analyzed to evaluate the degradation of chlorobenzene by P. chrysosporium. Results The degradation effects of P. chrysosporium on chlorobenzene under different conditions were investigated. The difference in the optimum temperature for the growth of the fungi and chlorobenzene degradation was observed. The data indicated that a lower temperature （28℃） would promote the degradation of chlorobenzene than the optimum temperature for the growth of the fungi （37℃）. A low nitrogen source concentration （30 mg N/L） had a better effect on degrading chlorobenzene than a high nitrogen source concentration （higher than 100 mg N/L）. A high initial concentration （over 1100 mg/m3） of chlorobenzene showed an inhibiting effect on degradation by P chrysosporium. A maximum removal efficiency of 95% was achieved at the initial concentration of 550 mg/m3. Conclusion P. chrysosporium has a rather good ability to remove gaseous chlorobeuzene. A low nitrogen source concentration and a low temperature promote the removal of chlorobenzene by P. chrysosporium. However, a high initial chlorobenzene concentration can inhibit chlorobenzene degradation.     

气相色谱法测定盐酸法舒地尔中有机溶剂残留量

目的建立气相色谱法测定盐酸法舒地尔中有机溶剂残留量的方法。方法采用气相色谱法,FID检测器,以毛细管色谱柱SE-54（30 m×0.53 mm,5.0μm）为分析柱。柱温为程序升温,用初始柱温55℃平衡0.5 min,以40℃/min的速度升温至70℃,平衡1 min,以40℃/min的速度升温至180℃,平衡3 min程序升温分别测定甲醇、二氯甲烷。用初始柱温50℃平衡3 min,以20℃/min的速度升温至180℃,平衡3min程序升温测定N,N-二甲基甲酰胺。载气为氮气,进样口温度200℃,检测器温度250℃。结果 3种有机溶剂完全分离,在所考察的浓度范围内具有良好线性关系,3个溶剂相关系数均大于0.999 0,甲醇、二氯甲烷、N,N-二甲基甲酰胺的检测限分别为0.065 7、1.100 0、0.016 6μg/mL,平均回收率分别为99.8%、98.4%、99.1%。结论本试验建立的方法简便灵敏,结果准确可靠,适用于盐酸法舒地尔原料药中有机溶剂残留量的检测。     

CN128中残留有机溶剂的顶空GC法测定

 目的  建立CN128原料药中8种有机溶剂残留量的测定方法。方法  采用顶空GC法, 色谱柱为Agilent HP-5 (30 m×0.25 mm, 0.25 μm), 柱温为程序升温:起始温度为35 ℃, 保持6 min, 以50 ℃/min升温至 110 ℃, 再以10 ℃/min升温至220 ℃, 保持3 min; 载气为氮气, 柱流速1.0 mL/min; 气化室温度200 ℃; FID检测器, 检测室温度250 ℃。有机溶剂检测项目为乙酸乙酯、二氯甲烷、乙醇、乙腈、正己烷、正庚烷、环己烷和氯化苄。结果  8种溶剂的线性关系、精密度、准确度均达到了《中国药典》2015版中残留溶剂限量规定的测定要求。结论  建立的方法能有效控制CN128原料药中乙酸乙酯、二氯甲烷、乙醇、乙腈、正己烷、正庚烷、环己烷和氯化苄的残留量。     

顶空气相色谱法测定双氢青蒿素磷酸哌喹片中乙醇残留

目的：建立一种气相色谱法用来测定双氢青蒿素磷酸哌喹片中乙醇残留量。方法：采用顶空自动进样气相色谱在DB-624（6%腈丙基苯基-94%二甲基硅氧烷,30 m×0.53μm×3.0μm）毛细管柱中进行测定,以正丙醇为内标物,氮气为载气,柱温：恒温80℃,保持10 min;流速：3.0 ml/min;分流比10∶1;进样口温度：220℃;检测器温度：220℃;顶空瓶平衡温度：80℃,保持30 min。结果：乙醇、正丙醇分离度良好,检测限（limit of detection,LOD）为0.19μg,定量限（limit of quantitation,LOQ）为0.57μg。乙醇含量在5.49～109.80μg范围内,线性关系良好,回归方程为：Y=0.002X＋0.003,r=0.999 9。平均回收率为95.63%,RSD=3.32%。结论：该方法可用于双氢青蒿素磷酸哌喹片中乙醇残留量的测定。     

LC-MS/MS法测定癫痫患者血浆中扑米酮的浓度

［摘要］ 〖HTH〗目的〖HTSS〗〖KG*2〗建立人血浆中测定扑米酮含量的高效液相色谱串联质谱（high performance liquid chromatography tandem mass spectrometry,LC-MS/MS）方法,并用于测定癫痫患者体内的血药浓度。 〖HTH〗方法〖HTSS〗〖KG*2〗色谱柱：Phenomenex Kinetex XB-C18（50 mm×3 mm,2.6 μm）。流动相：甲醇（A）-2%甲酸水（B）,进行梯度洗脱。流量：0.4 mL/min。柱温：40 ℃。进样量：5 μL。以咖啡因为内标,用电喷雾离子源进行正离子模式监测,多反应监测模式进行定量分析,源喷射电压5 500 V,离子源温度600 ℃。考察该方法的专属性、标准曲线及定量下限、精密度、回收率、稳定性及基质效应。选取20例临床口服扑米酮的癫痫患者（起始剂量为50 mg,1次/d;3 d后改为50 mg,2次/d;7 d后改为50 mg,3次/d;10 d后改为250 mg,3次/d）,于2周后清晨取静脉血2 mL。用LC-MS/MS法测定扑米酮的血药浓度。 〖HTH〗结果〖HTSS〗〖KG*2〗扑米酮在1~5 mg/L,最低定量下限为0.01 mg/L。平均回收率在95%以上,日间、日内精密度的相对标准偏差值均小于15%,稳定性良好。用该方法测定20例癫痫患者血样,其血药浓度范围为8.75~36.88 mg/L。 〖HTH〗结论〖HTSS〗〖KG*2〗本法方便、快捷、专属性好、敏感度高、结果准确,可用于测定癫痫患者血浆中的扑米酮浓度。     

甘蔗渣多糖脱蛋白方法研究

目的:比较Sevag法、酶法对甘蔗渣多糖脱蛋白的效果。方法:以蛋白脱除率、多糖含量为考察指标,选用Sevag法和酶法对甘蔗渣多糖进行脱蛋白处理。结果:进行8次Sevag法脱蛋白后蛋白的脱除率与多糖的含量分别达到77.47%、63.6%。酶法最佳条件下蛋白脱除率达到71.84%。结论:Sevag法进行8次脱蛋白对甘蔗渣多糖脱蛋白效果最佳;酶用量2%、温度50℃、时间3h对甘蔗渣多糖脱蛋白效果最佳。     

毛细管气相色谱法测定藿香正气软胶囊中百秋李醇的含量

目的建立毛细管气相色谱测定藿香正气软胶囊中百秋李醇含量的方法。方法样品经超声、离心后用毛细管气相色谱法测定。色谱条件:HP-5色谱柱(30 m×0.32 mm×0.25μm);初始温度170℃,保持3 min,以1℃/min的速度升至182℃,保持1 min,进样口温度280℃,检测器280℃,氮气流速0.6 mL/min。以正十八烷为内标,FID检测。结果百秋李醇在0.041 1~0.411 2 g/L浓度范围内,峰面积与内标峰面积之比值与浓度呈良好的线性关系(Y=2.94X+0.0128,r=0.999 2);平均回收率为98.96%,RSD=1.88%(n=6)。结论本方法准确、简便、灵敏、快速,可用于测定藿香正气软胶囊中百秋李醇的含量。     

加味藿香正气丸中百秋李醇的含量测定

目的:建立加味藿香正气丸中百秋李醇的GC含量测定方法.方法:色谱柱:非极性毛细管柱AT.SE-54(15 m×0.25 mm×0.33 μm);柱温采用程序升温:起始150℃,保持23 min,8℃/min升至230℃,保持2 min;进样口温度:280℃;检测器(FID)温度:280℃;载气:氮气,流速为1.0 mL...     

气相色谱法测定薄荷脑鼻用原位凝胶喷雾剂中薄荷脑的含量

目的 建立薄荷脑鼻用原位凝胶喷雾剂中薄荷脑含量的测定方法.方法 采用气相色谱法测定.色谱柱为AgilentDB-WAX毛细管柱(30 m×0.25 mm×0.25μm),柱温为120℃,检测器为氢火焰离子化检测器,检测器温度为260℃,进样口温度为220℃,进样量为1μl,载气为氮气,柱流速为1.0 ml/min.结果 薄荷脑质量浓度在0.02~0.20 mg/ml范围内具有良好的线性关系(r=0.9991);精密度、重复性、稳定性试验的RSD<2%;加样回收率为95.1%~103.4%,RSD为2.3%(n=6).结论 该方法操作简便、结果可靠、重复性好,可用于测定薄荷脑鼻用原位凝胶喷雾剂中薄荷脑含量.     

Heterogeneous photocatalytic degradation kinetic of gaseous ammonia over nano-TiO2 supported on latex paint film

Objective To investigate the photocatalytic degradation of gaseous ammonia in static state by using nano-TiO2 as photoeatalyst supported on latex paint film under UV-irradiation. Methods Experiments were conducted to study the relationship between the initial concentration of ammonia and the degradation products competing to be adsorbed on catalyst surface. Degradation of ammonia and its products were detected by spectrophotometry and catalytic kinetic spectrophotometry, respectively. Results On the one hand, TiO2 catalyst was excellent for degradation of ammonia, and the crystal phase of TiO2, anatase or ruffle, had little effect on degradation of ammonia, but the conversion of ammonia grew with the increase of catalyst content. On the other hand, apparent rate constant and conversion of ammonia decreased with the increase of initial concentration of ammonia, and the photocatalytic degradation reaction followed a pseudo-first-order expression due to-the evidence of linear correlation between -lnC/C0 vs. irradiation time t, but the relationship between initial concentration and the degradation products was not linear in low initial concentration. Conclusion Whether the photocatalytic degradation of ammonia in static state follows a first-order reaction depends on the initial ammonia concentration due to competition in adsorption between reactant and the degradation products.     

顶空-GC法检测灯盏花素中大孔树脂残留物的量

目的:建立灯盏花素中7种大孔树脂有机溶剂残留物的检测方法。方法:采用顶空进样毛细管气相色谱法,色谱柱为HP-INNOWAX毛细管柱(30 m×0.32 mm×0.5μm);柱温(程序升温):60℃维持16 min,再以每分钟20℃的升温速率升至200℃,维持2 min;进样口温度:240℃;FID检测器温度:300℃;2%的碳酸钠-25%二甲亚砜溶液为溶解介质,载气为氮气,测定三七总皂苷中正己烷、苯、甲苯、对二甲苯、邻二甲苯、苯乙烯、1,2-二乙基苯7种大孔树脂有机溶剂残留量。结果:本法线性关系良好,r=0.9938~0.9999,精密度RSDs均小于7.0%,7种溶剂的平均回收率为93.34%~98.39%,其RSDs在0.99~5.10%。结论:该方法操作简便快速,灵敏度高,准确度好,可作为灯盏花素中大孔树脂有机溶剂残留量的测定方法。     

GC法测定维吾尔药阿育魏果中麝香草酚的含量

目的：建立气相色谱法测定阿育魏果中麝香草酚的方法。方法采用气相色谱法对样品中麝香草酚进行定量分析,采用Agilent HP-5（30 m ＆#215;03．2 mm ,02．5μm）为色谱柱;以50℃作为初始柱温,恒温2 min ,再以10℃/min升温至230℃保持10 min。采用FID检测器,检测器温度为250℃,载气为氮气,柱流速为1 mL/min。结果麝香草酚进样量在浓度为02．0∽20．0 mg/mL（r ＝09．999）范围内与其峰面积呈良好线性关系。平均回收率为1004．7％（n ＝6）,RSD为16．0％。10批不同产地样品中麝香草酚的含量为18．84％∽33．11％,平均含量为24．44％。结论首次用GC色谱法对阿育魏果药材挥发性成分麝香草酚进行测定。GC法简便、精确,为有效制订质量标准提供科学依据。     

气相色谱法测定蒙药六味安消散中异土木香内酯的含量

目的：建立蒙药六味安消散（阿木日-6）中君药-土木香所含主要成分-异土木香内酯的含量测定方法,为蒙药六味安消散的质量控制提供科学依据。方法：采用美国Trace DSQⅡ型气相色谱仪,柱子：TR-WAX;柱箱温度：起始50℃,停留0 min,升温速率20℃/min,最终温度250℃,停留6 min,升温速率5℃/min,最终温度280℃,停留5 min;载气为氮气,流速为1 mL/min;进样口温度280℃;FID检测器,温度为300℃。结果：异土木香内酯在0.01-0.20 mg/mL范围内呈良好的线性关系,R2=0.9993,平均回收率为99.52%,RSD为2.00%。结论：该方法简便、快速、准确,重现性好,可为六味安消散的质量控制提供方法。     

排气通风笼具微环境的动态检测

目的 动态检测屏障环境中用于小鼠的新型排气通风笼具(EVC)的微环境指标.方法 测定两种饲养小鼠的EVC笼盒内通风风速和笼盒体积,计算笼盒换气次数.使用刨花垫料时换笼周期设置为7d,使用玉米芯垫料时换笼周期设置为14d,分别在每种换笼周期内每日连续检测笼盒内的噪声、压差、温度、相对湿度和氨浓度指标.结果 两种EVC笼盒内噪声分别为54.2士3.4 db和55.6士4.1 db,笼盒与屏障环境压差分别为-23.1±9.2 Pa和-27.5±11.6 Pa.从换笼周期第1日起,饲养小鼠的EVC笼盒内的温度差、相对湿度和氨浓度都呈现逐步升高的趋势;使用刨花垫料的两种EVC笼盒其第6日的氨浓度分别达到1.28±0.08 mg/m3和1.33±0.15 mg/m3,笼盒内温度分别为23.5±0.27℃和22.8±0.15℃,湿度分别为67.8％±2.2％和70.2％±1.1％;而使用玉米芯垫料的两种EVC笼盒内第12日达到氨浓度分别为1.95±0.46 mg/m3和2.17±0.33 mg/m3,笼盒内温度分别为23.8±0.4℃和24.1±0.2℃,湿度分别为70.3％±1.8％和69.6％±1.8％.结论 使用EVC笼盒饲养小鼠时,刨花垫料采取每6日换笼及玉米芯垫料采取每12日换笼的方案,可以使笼盒内的微环境指标:噪声、压差、温度、湿度和氨浓度,均符合国标GB 14925-2010要求.提示EVC与玉米芯垫料相结合,有助于维持笼盒内微环境稳定,可用于实验动物的生产和相关研究中.     

甲磺酸左氧氟沙星中有机溶剂残留量的气相色谱法测定

目的:建立甲磺酸左氧氟沙星中有机溶剂残留量的测定方法。方法:采用毛细管气相色谱法,色谱柱为HP-5毛细管柱(30m×0.32mm×0.25μm),柱温均为50℃,FID检测器,以N,N-二甲基甲酰胺为溶剂,载气为N2,进样口温度200℃,检测器温度300℃,分流比80:1,进样量1μL。结果:2种有机溶剂分离完全,且线性关系良好,线性范围分别为乙醇125.2～2003.2mg/L,正丁醇125.2～2002.4mg/L,乙醇和正丁醇的线性相关系数分别为0.9998和0.9996,平均回收率分别为99.54%、101.11%,最低检测限分别为7.1ng、11ng。结论:该方法灵敏、准确、可靠,适用于甲磺酸左氧氟沙星中有机溶剂残留量的检测。     

Microbial Degradation of Aniline by Bacterial Consortium

Objective To investigate the characteristics of microbial degradation of aniline by a stable bacterial consortium. Methods The bacterial consortium was isolated from activated sludge treating chemical wastewater using aniline as the sole source of carbon and nitrogen by enrichment and isolation technique. The biomass was measured as optical density (OD) at 510 nm using a spectrophotometer. Aniline concentrations were determined by spectrophotometer. The intermediates of aniline degradation were identified by GC/MS method. Results The bacterial consortium could grow at a range of aniline concentrations between 50 and 500 mg/L. The optimal pH and temperature for aniline degradation were determined to be 7.0 and 30, respectively. The presence of NH_4NO_3 as an additional nitrogen source (100-500 mg/L) had no adverse effect on bacterial growth and aniline degradation. The presence of heavy metal ions, such as Co~(2 ), Zn~(2 ), Ni~(2 ), Mn~(2 ) and Cu~(2 ) had an inhibitory effect on aniline degradation. Con     

Microbial degradation of aniline by bacterial consortium

Objective To investigate the characteristics of microbial degradation of aniline by a stable bacterial consortium. Methods The bacterial consortium was isolated from activated sludge treating chemical wastewater using aniline as the sole source of carbon and nitrogen by enrichment     

紫外光诱导选育高效降解苯酚的假单胞菌株

目的选育高效降解苯酚菌株,为环境酚污染的治理提供生物降解方法。方法以紫外线作诱变剂处理铜绿假单胞菌;用析因法优化降解条件。结果在苯酚浓度小于600mg／L,温度为35℃,pH值7.5时,历经12h,选育的假单胞菌诱变菌株（M3）能将苯酚完全降解;苯酚浓度高于600mg／L时,苯酚降解率随浓度的增高而降低。结论诱变菌株（N3）在一定的条件下对苯酚具有较好的降解效果。     

固定化微生物小球对水胺硫磷好氧降解的耐受性研究

固定化微生物小球对高浓度水胺硫磷的好氧降解有较好的耐受性。若进水的化学需氧量（ＣＯＤ（ｃｒ））为２１４５～１２５００ｍｇ／Ｌ，每隔４５ｄ左右用自来水冲洗４８ｈ，在室温下连续降解３７６ｄ并停止曝气１２２ｄ，然后再继续试验，所得ＣＯＤｃｒ去除率均在６０％左右。方差分析Ｐ＞０．０５，说明在整个试验期间，固定化微生物小球的活性无显著性差异。     

顶空GC法测定尿、血等生物检材中甲醇

目的：本文应用顶空GC法测定血、尿等生物检材中甲醇。方法：样品和标准均在60±2℃水浴中平衡10分钟,取上部气体气相色谱法测定。结论：本法最低检出浓度0．002mg／ml,线性范围0．002—0．05mg／ml,相关系数r＝0．9982。