UHPLC-Q/TOF MS结合HPLC-DAD定性和定量分析硫酸黏菌素可溶性粉中的未知添加物

定性和定量分析一批兽药硫酸黏菌素可溶性粉中的未知添加物。照《中国兽药典》2010年版一部对该批检品用微生物检定法进行含量测定时,发现该样品的抑菌圈为虚圈,用薄层色谱鉴别该样品,未显示与标准品溶液一致的主斑点,怀疑该样品中有处方外非法添加物。采用超高效液相色谱-四级杆-飞行时间质谱(UHPLC-Q/TOF MS)对该样品进行筛查,发现疑似添加物,并使用液相色谱-二极管阵列检测(HPLC-DAD)法进行了双重确证和含量测定。该样品中非法添加物确证为磺胺氯达嗪和甲氧苄啶,添加量分别为58.5 mg/g和13.4 mg/g。本研究通过建立筛查方法为监管部门提供技术支撑,通过分析非法添加物的可能原因为打击兽药处方外非法添加提供了思路。     

复方茵陈保肝口服液的制备与提取工艺研究

确定复方茵陈保肝口服液的制备工艺并建立质量标准。采用紫外分光光度法,以滨蒿内酯为对照品,在340 nm处测定按照不同工艺制备的口服液中香豆素含量,以香豆素含量高低作为优化标准。利用薄层色谱法对口服液中茵陈、党参、淫羊藿进行定性鉴别。用高效液相色谱法对口服液成品香豆素含量进行测定。口服液在料液比为1∶20,醇沉体积分数50%,煎煮时间2 h条件时香豆素含量最高。薄层色谱中斑点清晰,阴性对照无干扰。高效液相色谱法中滨蒿内酯在6.8~136μg范围内具有良好的线性关系,平均加样回收率为98.79%,RSD为1.39%。试验优化的制备工艺方法简单可行,建立的质量标准适用于复方茵陈保肝口服液的质量控制。     

耕作方式与长期定位施肥对雨养农田冬小麦产量的调控效应

为了明确西北黄土高原半湿润偏旱区耕作方式与长期定位施肥对冬小麦产量的调控效应,以设在半湿润偏旱区连续12年的耕作与肥料长期定位试验为平台,采用裂区设计,以传统耕作和免耕耕作为主处理,不施肥(CK)、单施无机氮肥(N)、单施无机磷肥(P)、单施有机肥(M)、无机氮磷肥配施(NP)、有机无机肥配施(NMP)为副处理,栽培制度为1年春玉米-3年冬小麦轮作,研究耕作及施肥措施对冬小麦产量的影响及其在生产年型间的变化关系。结果表明,不同年型及耕作方式均以有机无机配施冬小麦产量最高,有机肥单施高于化肥单施,磷肥单施高于氮肥单施。耕作方式间表现为传统耕作高于免耕耕作,年型间表现为丰水年>平水年>干旱年,耕作和施肥方式的增产效果以干旱年最好,平水年和丰水年差异不显著。有机无机配施与传统耕作结合优化了冬小麦冠层温度、叶绿素相对含量等生理指标,提高了光合速率、气孔导度及蒸腾速率,因而改善了有效穗、穗粒数和千粒重等产量性状而使冬小麦增产。在550 mm左右降水量的陇东旱塬雨养农业区,无论何种耕作方式及生产年型,长期采用有机无机或无机氮磷肥配施均表现出持续提高冬小麦产量的良好作用。因此,有机无机配施结合传统耕作是提高陇东半湿润偏旱区冬小麦产量的最佳耕作栽培模式。     

不同轮作序列对旱地胡麻土壤有机碳稳定性的影响

为了探索陇中黄土高原半干旱丘陵沟壑区胡麻轮作序列对土壤碳库的影响,2012-2016年通过4年定位试验,以连作为对照,研究了不同胡麻频率下的轮作序列(F:休闲;PWFW:25%Flax、马铃薯-小麦-胡麻-小麦;WFWP:25%Flax、小麦-胡麻-小麦-马铃薯;FWPF:50%Flax、胡麻-小麦-马铃薯-胡麻;WPFF:50%Flax、小麦-马铃薯-胡麻-胡麻;FFFF:100%Flax、胡麻-胡麻-胡麻-胡麻)对土壤团聚体、总有机碳(TOC)、土壤颗粒有机碳(POC)、土壤微生物碳(MBC)和氮(MBN)的影响。结果表明,休闲、不同轮作序列和低胡麻频率显著增加了030 cm土层<0.25 mm粒级的土壤团聚体含量、TOC和POC含量,而随胡麻频率的增加三者的含量呈下降趋势。其中,25%Flax处理下土壤团聚体含量较播前和休闲处理分别显著增加了2.02%4.04%和9.56%11.73%;土壤有机碳(SOC)较连作显著增加5.95%7.48%。50%Flax处理下胡麻位置对土壤SOC影响显著,且轮作(FWPF)显著高于连作(WPFF)。060 cm土层土壤SOC含量表现为休闲>播前≈25%Flax>50%Flax>100%Flax。与连作相比,轮作显著提高了010 cm土层土壤TOC和POC含量,呈现表层富集现象。土壤POC含量表现为25%Flax≈休闲>50%Flax>100%Flax。此外,轮作换茬显著增加了土壤MBC含量,且随着胡麻频率的增加,030 cm土层土壤MBC含量逐渐降低。与播前、休闲、轮作相比,连作显著降低土壤微生物碳氮比,50%Flax(WPFF)轮作序列和土层深度对土壤有机碳和微生物量的互作效应显著。综合来看,休闲可以显著改善土壤理化性状,25%胡麻频率的轮作序列利于保持土壤团聚体稳定性,增加土壤TOC、SOC和POC含量,而50%Flax轮作序列(WPFF)能够提高土壤微生物量和微生物碳氮比。表明25%胡麻频率的轮作序列均可维持土壤有机碳的稳定性,是旱地胡麻比较理想的轮作序列。     

土壤易氧化有机碳与溶解性有机碳对荒漠草地沙漠化过程中土壤碳库变异的表征

以干旱、半干旱地区荒漠草地不同沙漠化阶段土壤为研究对象,研究不同沙漠化阶段土壤易氧化有机碳与溶解性有机碳含量和分配比例变异规律,分析不同沙漠化阶段土壤碳库指数变化,探讨荒漠草地沙漠化过程中土壤易氧化有机碳与溶解性有机碳对土壤碳库的表征作用。结果表明,随着荒漠草地沙漠化程度的加剧,易氧化有机碳含量表现出一定的波动性,但整体呈下降趋势,溶解性有机碳含量呈线性下降。易氧化有机碳和溶解性有机碳分配比例均在荒漠草地达到最大值,在半固定沙地达到最小值。利用易氧化有机碳含量计算的土壤碳库管理指数随荒漠草地沙漠化程度增加表现出先下降后上升趋势,利用溶解性有机碳含量计算的土壤碳库管理指数呈线性下降趋势。易氧化有机碳、溶解性有机碳含量与土壤有机碳均显著正相关,但溶解性有机碳的相关系数略高于易氧化有机碳。通过比较活度敏感指数和碳库管理指数敏感指数发现,荒漠草地逆向演替至固定沙地过程中,易氧化有机碳的各项敏感指数均高于溶解性有机碳。固定沙地演替至流动沙地过程中,溶解性有机碳的各项敏感指数均高于易氧化有机碳,表明易氧化有机碳能够较好地表征荒漠草地沙漠化前期土壤碳库变化,而荒漠草地沙漠化中期和后期利用溶解性有机碳表征效果更好。     

Pharmacokinetics of articaine hydrochloride and its metabolite articainic acid after subcutaneous administration in red deer (Cervus elaphus)

AIM: To develop and validate a simple and sensitive method using liquid chromatography-mass spectrometry (LC-MS) for quantification of articaine, and its major metabolite articainic acid, in plasma of red deer (Cervus elaphus), and to investigate the pharmacokinetics of articaine hydrochloride and articainic acid in red deer following S/C administration of articaine hydrochloride as a complete ring block around the antler pedicle.

METHODS: The LC-MS method was validated by determining linearity, sensitivity, recovery, carry-over and repeatability. Articaine hydrochloride (40?mg/mL) was administered S/C to six healthy male red deer, at a dose of 1?mL/cm of pedicle circumference, as a complete ring block around the base of each antler. Blood samples were collected at various times over the following 12 hours. Concentrations in plasma of articaine and articainic acid were quantified using the validated LC-MS method. Pharmacokinetic parameters of articaine and articainic acid were estimated using non-compartmental analysis.

RESULTS: Calibration curves were linear for both articaine and articainic acid. The limits of quantifications for articaine and articainic acid were 5 and 10?ng/mL, respectively. Extraction recoveries were >72% for articaine and >68% for articainic acid. After S/C administration as a ring block around the base of each antler, mean maximum concentrations in plasma (C_max) of articaine were 1,013.9 (SD 510.1) ng/mL, detected at 0.17 (SD 0.00) hours, and the C_max for articainic acid was 762.6 (SD 95.4) ng/mL at 0.50 (SD 0.00) hours. The elimination half-lives of articaine hydrochloride and articainic acid were 1.12 (SD 0.17) and 0.90 (SD 0.07) hours, respectively.

CONCLUSIONS AND CLINICAL RELEVANCE: The LC-MS method used for the quantification of articaine and its metabolite articainic acid in the plasma of red deer was simple, accurate and sensitive. Articaine hydrochloride was rapidly absorbed, hydrolysed to its inactive metabolite articainic acid, and eliminated following S/C administration as a ring block in red deer. These favourable pharmacokinetic properties suggest that articaine hydrochloride should be tested for efficacy as a local anaesthetic in red deer for removal of velvet antlers. Further studies to evaluate the safety and residues of articaine hydrochloride and articainic acid are required before articaine can be recommended for use as a local anaesthetic for this purpose.     

Response of labile organic C and N pools to plastic film removal from semiarid farmland soil

To examine the effects of plastic film removal on grain yield and soil organic matter (SOM), a spring maize (Zea may L.) field experiment was conducted for 5 yr at Changwu Agricultural and Ecological Experimental Station of Northwest China. Compared with traditional plastic film mulching during entire growing stages (FM), plastic film removal at the silking stage (RM) resulted in a 6.3% higher average maize yield. Under the RM treatment, soil organic carbon and total nitrogen significantly increased after the 5‐yr cultivation in the 0‐ to 20‐cm layer. Significant increases in extractable organic C (EOC), KMnO₄‐oxidizable C (KMnO₄‐C) and C management index (CMI) in the 0‐ to 20‐cm layer, and light fraction organic C and EOC in the 20‐ to 40‐cm layer were observed in response to plastic film removal after the 1‐yr treatment; the responses were more significant after 5 yr. Under the RM treatment, significant increases in microbial biomass C, light fraction organic N, extractable organic N, KMnO₄‐C and CMI were also observed after five years in the 20‐ to 40‐cm layer. Moreover, KMnO₄‐C and EOC were much more sensitive than other labile SOM fractions to the application of RM, even after only 1 yr of cultivation. Therefore, compared with mulching for the whole growing season, plastic film removal at the maize silking stage is an effective option for increasing yields and enhancing SOM concentration and soil sustainability in the regions with semiarid monsoon climates that have sufficient rainfall during maize reproductive stages.     

Proton accumulation accelerated by heavy chemical nitrogen fertilization and its long-term impact on acidifying rate in a typical arable soil in the Huang-Huai-Hai Plain

Cropland productivity has been signiifcantly impacted by soil acidiifcation resulted from nitrogen (N) fertilization, especialy as a result of excess ammoniacal N input. With decades’ intensive agricul...     

农五师葡萄钾素动态变化及调节措施研究

通过叶分析研究了不同葡萄品种叶柄全钾5～9月含量动态变化规律.结果表明:葡萄叶柄钾含量在生育期内整体呈波浪式下降趋势,前期下降迅速,中期平缓,进入浆果成熟期后又趋于下降；强势品种在整个生长季节内对钾的吸收大于弱势品种；早熟品种叶柄内钾含量变化趋势比晚熟品种提前.根据新疆农五师葡萄园区土壤有效钾含量分布现状,建议生产中应根据葡萄钾元素动态变化特点,不同团场应结合当地土壤有效钾含量相应补充.     

不同生态因子对荚果蕨生长和光合特性的影响

为研究荚果蕨抗逆性生理机制并且为荚果蕨栽培提供理论依据和参考,以荚果蕨为实验作物,利用盆栽法、光合作用测定仪、土壤农化分析方法研究了荚果蕨生长及光合特性对土壤质量含水量、有机肥料、光照强度等生态因子的响应机制。研究结果表明:荚果蕨幼苗对于水分胁迫具有一定的抗逆性,土壤质量含水量为田间持水量的70%~75%时荚果蕨叶片长度最大,净光合速率(Pn)与蒸腾速率(Tr)表现为随着土壤含水量的增加先上升后下降,水分利用效率(Ew)变化趋势与之相反;不同有机肥料间比较腐熟猪粪肥培肥效果较好,且在1500 kg/hm2施用量时效果达到峰值;各遮阳措施均有利于荚果蕨生长,实验处理为使用透光率为30%的遮阳网时荚果蕨叶片长度最佳。荚果蕨最适宜生长条件为:土壤质量含水量为田间持水量的70%~75%;施用腐熟猪粪肥1500 kg/hm2;遮阳措施透光率为30%。