Free and HF-HO-extractable amino acids determined by high performance liquid chromatography in a loamy sand soil

Summary Amino acids were extracted from fertility plots of a loamy sand soil with 0.05 M HF-HCl and with a 10% ethanol solution (free amino acids) and analysed by reverse-phase high performance liquid chromatography (HPLC). The total quantities of amino-N compounds analysed were 4.4 g/g soil for the acid treatment and 22.6 g/g soil for the 10% ethanol extract. Glycine and glutamic acid were the most abundant of 15 amino-N compounds in the HF-HCl extracts, whereas glutamic acid and ornithine + NH⁺ ₄ were found in the highest concentration in the 10% ethanol extracts. The HF-HCI pretreatment is used to increase the efficiency of the extraction of soil organic matter. Although this pretreatment removed some amino acids, the acids extract less than 1% of the total amino-N content of the crude soil extracts. The pretreatment, therefore, was not overly destructive. Comparisons between the amino acids extracted from the fertility plots were not conclusive, except for glycine, which was greater in concentration in the higher fertilizer N plots of the same crop rotation.     

高效液相色谱法测定土壤中的二氯喹啉酸

用50 ml甲醇︰0.05 mol/L硼砂溶液(p H=10)(9︰1,v/v)作为提取剂对20 g(或适量)土壤样品中残留的二氯喹啉酸振荡提取2 h,离心过滤后分取滤液25 ml浓缩,甲醇定容至2 ml,再用滤膜过滤后待测定;高效液相色谱仪(HPLC)以1.0 ml/min的甲醇︰1%乙酸水溶液(55︰45,V/V)为流动相,柱温45℃,在238 nm的紫外光波长下进行二氯喹啉酸的外标法定量。该方法精密度为6.0%,检出限为0.012 mg/kg,不同类型土壤的加标回收率74.9%~98.8%,能满足有机分析要求。该方法既简捷易操作,又能满足土壤中二氯喹啉酸低残留量的测定。     

Enzymatic activities in constructed wetlands and di-n-butyl phthalate (DBP) biodegradation

The bioaccumulation of phthalate acid esters (PAEs) from industrial products and their mutagenic action has been suggested to be a potential threat to human health. The effects of the most frequently identified PAE, Di-n-butyl phthalate (DBP), and its biodegradation, were examined by comparison of two small scale plots (SSP) of integrated vertical-flow constructed wetlands. The influent DBP concentration was 9.84 mg l⁻¹ in the treatment plot and the control plot received no DBP. Soil enzymatic activities of dehydrogenase, catalase, protease, phosphatase, urease, cellulase, β-glucosidase, were measured in the two SSP after DBP application for 1 month and 2 months, and 1 month after the final application. Both treatment and control had significantly higher enzyme activity in the surface soil than in the subsurface soil (P<0.001) and greater enzyme activity in the down-flow chamber than in the up-flow chamber (P<0.05). In the constructed wetlands, DBP enhanced the activities of dehydrogenase, catalase, protease, phosphatase and inhibited the activities of urease, cellulase and β-glucosidase. However, urease, cellulase, β-glucosidase activities were restored 1 month following the final DBP addition. Degradation of DBP was greater in the surface soil and was reduced in sterile soil, indicating that this process may be mediated by aerobic microorgansims. DBP degradation fitted a first-order model, and the kinetic equation showed that the rate constant was 0.50 and 0.17 d⁻¹, the half-life was 1.39 and 4.02 d, and the r² was 0.99 and 0.98, in surface and subsurface soil, respectively. These results indicate that constructed wetlands are able to biodegrade organic PAEs such as DBP.     

HPLC在化学生态学和环境监测中的应用

高效液相色谱（HPLC）是在20世纪60年代末期，在经典液相色谱法和气相色谱法的基础上发展起来的新型分离分析技术。本文对其近期在化学生态学和环境监测中的应用做了评述。     

HPLC法测定白头翁中皂苷B4含量及其中药材标准化研究

目的：建立HPLC测定白头翁药材中白头翁皂苷B4含量的方法,并比较不同产地、不同生长年份对白头翁皂苷B。含量的影响,以评价白头翁药材质量。方法：HPLC流动相：乙晴：水（28：72）;流速：1．0mL／min;分离柱采用ZORBAXSB—C1B（4．6mm&#215;150mm,5μm）,反相填料;柱温：室温;检测波长：205nm。结果：皂苷B4进样量在0．3125—10μg范围内与吸收峰面积呈良好的线性关系（r=0．9995,n=6）,平均加样回收率为99．74％,RSD=3．28％（n=3）。结论：该方法简便、准确、重现性好,可用于白头翁皂苷B4的含量测定;白头翁中皂苷B4含量以安徽风阳产药材较高,可作道地药材。     

口服不同剂型替米考星在鸡体内相对生物等效性研究

本试验按单剂量口服的方法对健康蛋鸡进行替米考星可溶性粉和替米考星溶液中主要组分替米考星的生物利用度和药代动力学研究。利用HPLC方法分析不同时间点试验鸡血浆中的药物浓度。药物的药动学参数结果显示,替米考星可溶性粉和替米考星溶液的平均血药浓度-时间曲线下面积(AUC0-48)分别为(16.947±0.624)μg/mL.h和(16.020±0.631)μg/mL.h,没有显著差异;二者AUC0-48比值为1.058,Cmax分别为(0.759±0.012)μg/mL和(0.764±0.012)μg/mL,比值为0.993;替米考星可溶性粉和替米考星溶液的t1/2β、C l(s)、t1/2 Ka和V/F(c)均没有显著差异;二者的tmax分别为(1.211±0.036)h和(1.030±0.063)h虽然有显著差异,但并不能以此说明二者生物学的非等效性。试验结果说明,单剂量口服替米考星可溶性粉和替米考星溶液后,替米考星被迅速吸收,消退缓慢,依据生物等效性的重要评判指标,得出替米考星可溶性粉和替米考星溶液在治疗中可以相互替代。     

采用HPLC法检测鸡组织中尼卡巴嗪残留量

建立了鸡组织(肌肉、肝脏、肾脏)中尼卡巴嗪残留的高效液相色谱检测方法。鸡组织样品经乙腈提取,正己烷液-液萃取,碱性氧化铝小柱固相萃取净化,三氯甲烷淋洗后以甲醇-乙腈(90/10,v/v)洗脱,洗脱液浓缩后以流动相溶解,过滤。选用ODS高效液相色谱柱进行色谱分析,流动相为乙腈-水(50/50,v/v),紫外检测波长340 nm。DNC标准品工作液在0.04~10.0 mg/L浓度范围内线性关系良好(r=0.999 9)。组织中药物添加浓度分别为0.1 mg/kg、0.2 mg/kg、0.4 mg/kg时,肌肉样品中药物平均回收率为(80.21±0.95)%;肝脏样品中药物平均回收率为(75.37±5.04)%;肾脏样品中药物平均回收率为(78.84±2.78)%。日内、日间变异系数分别低于7%和10%。在该检测条件下,检测限可以达到0.02 mg/kg。     

HPLC测定狼牙刺不同组织器官中氧化槐果碱含量

建立了采用高效液相色谱法测定狼牙刺Sophra viciifolia中氧化槐果碱含量的方法：色谱柱为ZORBAX C18柱（4.6 mm×150 mm,5 μm）;流动相0.04 mol/L磷酸溶液（pH值1.8）-甲醇（体积比90∶10）;流速1.0 mL/min;检测波长220 nm;柱温20 ℃。测定了狼牙刺不同组织器官中氧化槐果碱含量,结果表明：狼牙刺植物花蕾中氧化槐果碱含量最高,达2.114%,其次是幼果、种子、花、叶、当年生幼茎,氧化槐果碱含量分别为1.735%、1.651%、1.615%、0.540%和0.244%,多年生茎含量最低,只有0.045%。该结果对狼牙刺资源的开发利用及生态保护具有积极意义。     

复合维生素中呋喃类违禁药物高效液相色谱检测方法研究

为了快速检测呋喃类违禁药物,本文研究了复合维生素中呋喃唑酮、呋喃西林和呋喃妥因3种呋喃类违禁药物的高效液相色谱(HPLC)检测方法,建立了同时检测呋喃唑酮、呋喃西林和呋喃妥因的定性、定量方法.采用反相高效液相色谱(RP-HPLC)法,参考色谱条件:色谱柱为Alltech C18柱250mm×4.6mm(i.d.),5 μm;流动相为乙腈-水(28:72,V/V);流速为1.0 mL/min;检测波长为365 nm;柱温为室温;进样量为10 μL.结果表明,呋喃唑酮、呋喃西林和呋喃妥因的加样平均回收率分别为:96.1%、99.7%、99.9%;线性方程:呋喃唑酮y=4×109x+233505,相关系数R2=0.9993;呋喃西林y=5×109x+253168,相关系数R2=1;呋喃妥因y=5×109x+201638,相关系数R2=1.这表明,本实验建立的测定方法简便、灵敏、准确、快速、重现性好,可用于复合维生素中呋喃类违禁药物的定性和定量检测.