高效液相色谱法测定青贮饲料桑中的乳酸、乙酸和丙酸含量条件探讨

本文应用高效液相色谱法（HPLC）对青贮饲料桑中的乳酸、乙酸和丙酸含量测定进行了研究。通过对色谱柱、流动相、流速及样品处理条件进行优化，建立了一种应用HPLC法同时测定青贮饲料桑中乳酸、乙酸和丙酸含量的方法。研究结果表明：乳酸、乙酸和丙酸在一定浓度下具有良好的线性关系，且相关系数R2均大于0.999，加标回收率为98.35% ~ 104.24%，标准品中回收率和精密度试验相对标准偏差（RSD）为0.01%~0.58%，表明该方法准确性较好。3种物质检出限为4.928 ~ 9.489 mg/L，适用于青贮饲料桑中有机酸的定量检测。 [关键词] 高效液相色谱（HPLC）|青贮饲料桑|乳酸|乙酸|丙酸     

超声提取-离子色谱法测定芹菜中氯量

研究了超声提取-离子色谱法测定芹菜中氯含量的方法。芹菜经超声提取20 min后,以浓度4.5 mmol/L Na₂CO₃和0.8 mmol/L NaHCO₃为淋洗液,经IonPacAG23分离测定。本方法具有快速、灵敏、准确度高,适合于芹菜中氯量的测定。     

Role of IP3R in LH-EGFR-induced mouse oocyte meiotic resumption

AIM: To explore the effect of inositol 1, 4, 5-trisposphate receptor (IP₃R) in luteinizing hormone-epidermal growth factor receptor (LH-EGFR)-induced oocyte meiotic resumption. METHODS: Models of mouse cumulus-oocyte complexs (COCs) culture and follicle culture in vitro were generated to study the effects of 2-aminoethyl diphenyl borate (2-APB) and heparin (IP₃R specific inhibitors) on LH/EGF-induced oocyte meiotic resumption and EGF-induced cumulus cell expansion. Real-time PCR was used to detect the mRNA expression of cumulus expansion-related factors. The changes of the intracellular calcium level were monitored using Fluo 3-AM, and the cGMP level was measured by ELISA. RESULTS: The inhibitors of IP₃R, 2-APB and heparin, dramatically reversed EGF-induced oocyte maturation (P<0.05) and decreased cGMP levels in COCs (P<0.05). In addition, 2-APB and heparin reversed EGF-induced cumulus expansion, and significantly inhibited EGF-induced cumulus expansion-related factor expression (P<0.05). The activation of IP₃R increased intracellular calcium level, and the study found that 2-APB and heparin dramatically reversed EGF-induced elevation of calcium level in cumulus cells (P<0.05). Follicular culture in vitro showed that 2-APB and heparin significantly reversed the LH-induced oocyte maturation (P<0.05). CONCLUSION: LH-EGFR signaling pathway increases calcium level in cumulus cells through IP₃R, resulting in meiotic resumption.     

偏高岭土对高强机制砂混凝土性能的影响

利用扫描电子显微镜(SEM)、压汞法(MIP)、快速氯离子迁移系数法(RCM)等手段,研究了偏高岭土(MK)掺量对高强机制砂混凝土抗压强度以及抗氯离子渗透性能的影响.研究发现: 掺入MK能够有效改善高强机制砂混凝土的力学性能和抗氯离子渗透性能:随MK掺量增加,抗压强度与抗氯离子渗透性能均呈先增大后减小的趋势,最佳MK掺量为8%,此时28 d抗压强度为98.5 MPa,较基准组增加13%,氯离子迁移系数为1.89×10^-12 m²/s,较基准组减小60%.微观结构试验表明适宜的偏高岭土掺量能够有效促进水泥水化;偏高岭土颗粒的晶核效应和微集料填充效应协同作用,使得机制砂混凝土的微观结构更加均匀密实,机制砂混凝土的多害孔、有害孔减少,少害孔增加,从而提高了机制砂混凝土抗压强度和抗氯离子渗透性能.     

超高效液相色谱-串联质谱法测定饲料中的二氢吡啶

【目的】二氢吡啶是一种新型的饲料添加剂,具有促进动物生长、提高饲料利用率、改善肉质等功效,目前已在畜牧生产中得到广泛应用。然而,二氢吡啶并不是允许使用的药物饲料添加剂,其在饲料中高水平添加所带来的畜产品中二氢吡啶残留可引起敏感人群严重的低血压反应。央视3.15晚会曝光了部分饲料企业违规使用二氢吡啶、硫酸黏杆菌素、喹乙醇等兽药,引起社会的广泛关注和政府的高度重视,因而亟需建立饲料中二氢吡啶的检测方法,为饲料企业合理用药和政府监管提供必要的技术支撑。【方法】采用UPLC上常用的BEH C18色谱柱,分别使用甲醇-水、乙腈-水、甲醇-0.1%甲酸、乙腈-0.1%甲酸作为流动相,优化了不同组成和比例流动相对色谱分离和质谱电离的影响。在正离子模式下进行母离子扫描,确定准分子离子,优化仪器毛细管电压、锥孔电压、雾化气流速等参数;然后进行子离子扫描,优化碰撞能量、驻留时间等参数,以确定丰度较高的两个子离子作为定性离子,并选择其中丰度最高的作为定量离子。比较甲醇、乙腈等不同溶剂对提取效率的影响,以及C18、HLB、MCX和碱性氧化铝等固相萃取柱(SPE)对净化效果的影响,确定较优的样品前处理方法。【结果】优化确定了较佳的前处理方法:采用乙腈超声提取,提取液在60℃下氮气吹干,残余物用乙腈﹕水(1﹕9,v/v)复溶,过HLB固相萃取柱净化,用乙腈﹕水(9﹕1,v/v)洗脱,洗脱液过0.22μm有机滤膜后上超高效液相色谱-串联质谱仪(UPLC-MS/MS)测定。采用电喷雾离子源,在多反应监测(MRM)模式下,二氢吡啶的[M+H]+为m/z 254,失去乙氧基(CH3-CH2-O+,46 Da)后产生主要的碎片离子m/z 208,m/z 208脱掉羰基(C=O,28 Da)产生碎片离子m/z 180,m/z 180进一步脱去乙酯基(CO-O-CH2-CH3,73 Da)后得到碎片离子m/z 108,因此本研究以离子对m/z 254208为定量离子,m/z 254180为定性离子。以0.1%的甲酸水-乙腈为流动相进行梯度洗脱,在10 min内完成了二氢吡啶的分离,且峰形尖锐,灵敏度高。二氢吡啶在0—500μg·L~(-1)浓度范围内呈现良好的线性关系(R2≥0.9992),根据20个空白样品的基线噪音,取其平均值,以信噪比(S/N)=3为检出限(LOD),S/N=10为定量限(LOQ),二氢吡啶的LOD、LOQ分别为10和50μg·kg-1。在10、50和100μg·kg-1三个添加水平下,二氢吡啶的平均回收率为82.6%—101.0%,日内变异系数为0.8%—6.7%,日间变异系数为4.7%—9.2%。【结论】该方法操作简便、快速、稳定,适用于饲料中二氢吡啶的日常监测。     

Balance and concentration of nitrogen and potassium affect growth and nutrient status in soilless cultivated lisianthus

Purpose: Nitrogen (N) / potassium (K) nutrient balance has been studied for some ornamental plants, however, available information is limited. Here we investigate the optimum N and K balance and concentration for lisianthus production in soilless medium.

Materials and methods: The effect of three N / K balances: 1.43, 2.14 and 4.29, prepared by varying the concentration of N and K, were evaluated in lisianthus grown in soilless medium (volcanic rock).

Results: Plants fertigated with a N / K balance of 2.14 exhibited enhanced height and stem dry weight when compared to plants fertigated with a balance of 4.29, and a higher flower buds count and total dry weight than those fertigated with a balance of 1.43 or 4.29. Plants fertigated with a balance of 2.14 exhibited increased dry weight when N was reduced from 15 to 9?meq?L^?1 and K from 7 to 4.2?meq?L^?1, suggesting that lisianthus does not require high levels of these nutrients. Although shoot N concentration was not correlated with N concentration in the nutrient solution or balance, increasing N in the shoot was associated with higher P and Mg in the plant tissues. In general, P, Ca, and Mg in plant tissues were unaffected by the external N / K balance, however, the internal P and Mg concentrations were positively correlated with shoot dry weight. Shoot K concentration significantly increased when the N / K balance decreased, which is related to the higher concentrations of external K when the balance decreased.

Conclusions: The optimum N / K balance for lisianthus was 2.14. However, there was a concentration effect, as fertigation with solutions containing a N / K balance of 2.14 and an N and K concentration of 9 and 4.2?meq?L^?1 respectively, resulted in plants with the greatest dry weight.     

Lippia alba (Verbenaceae) hydrolate as sedative of tambaqui (Colossoma macropomum) juveniles in simulated transport conditions

Lippia alba hydrolate (LAH) is produced as a secondary product in essential oil extraction. The objective of this study was to evaluate the use of LAH in a simulation of the transport of tambaqui (Colossoma macropomum) juveniles. A series of 17 hr simulations were performed using load densities of 30, 60 and 90 juveniles per L and four LAH concentrations of 0.4%, 1%, 2% and 5%, with a control of just water. Fish survival, temperature, dissolved oxygen, conductivity, pH, ammonia excretion, alkalinity water hardness and net Na⁺, K⁺, Cl^‐ fluxes, were all evaluated before and after the transport simulations. Mucous cell densities in the gills were also determined microscopically, post simulation. The results showed that addition of 5% LAH achieved better survival during the simulation than the water control. Dissolved oxygen was significantly lower with an increased load density. Also, conductivity, NH₄ excretion and net ionic fluxes (K⁺ and Cl^?) were lower with 5% LAH, although mainly where higher load densities were tested. Mucous cell density was lower in LAH concentrations of 2% and 5%, again with higher load densities. In view of these findings, it is suggested that 5% LAH is an effective sedative for use in the transport of tambaqui, mainly with high load densities. This work is the first study of LAH and highlights its potential applications in aquaculture management.     

Cu2+和Zn2+在土壤电场中的极化对黑土胶体凝聚的影响

金属离子在土壤胶体固-液界面上的行为差异引起土壤胶体絮凝过程的差异,并深刻影响土壤溶液中养分或污染物的迁移转化。为明确Cu~(2+)和Zn~(2+)两种金属离子界面行为对土壤胶体凝聚的影响,本文选取黑土胶体为研究对象,利用动态/静态光散射技术研究专性吸附离子Cu和Zn体系中不同离子浓度条件下黑土胶体的凝聚行为。结果表明:(1)Cu~(2+)和Zn~(2+)两种金属离子引发黑土胶体凝聚的机制相似,均是低浓度下的慢速凝聚和高浓度下的快速凝聚,达到快速凝聚机制后,胶体的总体平均凝聚速率受离子种类影响较小。(2)Cu~(2+)对黑土胶体聚沉能力大于Zn~(2+),Zn~(2+)的临界聚沉浓度是Cu~(2+)的3.51倍,在黑土胶体的凝聚过程中存在强烈的离子特异性效应。(3)两种离子体系中颗粒间相互作用的活化能差异随离子浓度的降低而增大。此两种离子在凝聚作用的较大差异性源于Cu~(2+)较Zn~(2+)对有机配位体有较强的亲和力,以及黑土胶体表面附近强电场对离子的强烈极化作用扩大了两种离子本身的微小差异。     

崇礼区典型林分空气负离子浓度及影响因素

[目的]对崇礼区3种主要林分类型的空气负离子浓度变化规律以及影响因素进行研究,为该地生态效益评估以及生态旅游规划提供依据。[方法]本研究通过对崇礼区典型林分类型空气负离子浓度进行连续观测,并以开阔无林地为参照对象,采用柱状图、散点图、回归分析等方法研究河北杨(Populus hopeiensis,PHF)、白桦(Betula platyphylla,BF)和油松(Pinus tabulaeformis,PF,)3种纯林以及无林地(NF)空气负离子浓度日变化特征,分析气象因素及植物光合特性对空气负离子的影响,并运用单极系数法以及空气质量系数法对不同林分空气质量进行评价。[结果]表明:(1)空气负离子浓度变化趋势呈双峰型,最低值一般出现在中午,不同林分最高值出现时间不同。不同林分空气负离子浓度具有明显差别,空气负离子浓度从高到底依次为:河北杨(1 101 ion·cm-3)白桦(847 ion·cm-3)油松(755 ion·cm-3)无林地(344 ion·cm-3)。(2)不同林分空气负离子浓度与气温呈负相关,与相对湿度呈正相关;不同林分空气负离子浓度与植物光合特性总体呈正相关。(3)计算空气质量评价参数得出不同林分单极系数从小到大依次为河北杨(0.92)油松(1.01)白桦(1.25)无林地(1.37),各林分空气质量评价指数从大到小依次为河北杨(1.25)白桦(0.85)油松(0.80)无林地(0.27)。[结论]不同林分空气负离子浓度存在差异且阔叶林高于针叶林,空气离子浓度的变化受外界气候因素及自身植物光合特性的影响明显,不同林分空气质量评价指数也存在差异,合理配置林分资源有利于空气质量提升。     

贴敷类医疗器械产品中非法添加樟脑、薄荷脑、冰片的情况分析

目的 检测26家企业34批次的贴敷类医疗器械产品中的樟脑、薄荷脑、冰片，为制订产品标准或补充检验方法提供参考。方法 采用气相色谱法对贴敷类医疗器械产品中的樟脑、薄荷脑、冰片进行初筛，再采用气-质联用法（GC-MS）对结果进行确证。结果 34批样品中樟脑、薄荷脑、冰片，10批次全部检出，3批次全部未检出，21批次部分检出。34批样品中樟脑共26批次检出；薄荷脑共22批次检出；冰片共18批次检出。结果未表明明显地域差异。结论 贴敷类医疗器械产品中樟脑、薄荷脑、冰片的添加情况非常普遍，形势较为严峻，建议补充该类产品非法添加樟脑、薄荷脑、冰片的法定检验方法，为产品质量控制、分类界定和行政执法提供技术支持。