Residues of enrofloxacin, furazolidone and their metabolites in Nile tilapia (Oreochromis niloticus)

The residues of enrofloxacin and its metabolite in Nile tilapia (Oreochromis niloticus) were studied after oral dose of 50 mg/kg for 7 days. To find the differences between Nile tilapia and Chinese shrimp (Penaeus chinensis), the residues of enrofloxacin in P chinensis were also studied under the same conditions. The results showed that enrofloxacin metabolized into ciprofloxacin in both Nile tilapia and P chinensis, the maximal concentration of enrofloxacin in muscle, liver and plasma of Nile tilapia were 3.61 mu g/g, 5.96 mu g/g, 1.25 mu g/ml respectively, and ciprofloxacin in muscle was 0.22 mu g/g. The maximal concentration of enrofloxacin and ciprofloxacin in P chinensis were 1.68 mu g/g and 0.07 mu g/g respectively. The predicted withdrawal time for Nile tilapia was 22 days, and P. chinensis was 12 days under our experiment conditions. The residues of fitrazolidone [3-(5-nitrofurfurylidenamino)-2-oxazolidinone] and its main metabolite 3-amina-2-oxazolidinone (AOZ) in Nile tilapia were first determined by HPLC/MS. Results showed that after oral dose of 30 mg/kg for 7 days, the maximum concentration of farazolidone in Nile tilapia was 413 mu g/kg after 6 h, whereas AOZ residue reached its maximum (31 mu g/kg) right after stopping treatment. In contrast to the high metabolic rate of furazolidone, AOZ was very difficult to eliminate in vivo, thus the withdrawal time of furazolidone in Nile tilapia was 22 days at least. (c) 2005 Elsevier B.V. All rights reserved.

Simultaneous Determination of Multi-Organotin Compounds in Seawater by Liquid-Liquid Extraction-High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

The hyphenated technique of high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry (HPLC-ICP-MS) was applied to the simultaneous determination of five organotin compounds (trimethyltin, dibutyltin, tributyltin, diphenyltin and triphenyltin) in seawater samples. Agilent TC-C18 column was used for the separation, the mobile phase of HPLC was CH3CN : H2O: CH3COOH=65 : 23 : 12 (phi), 0.05% TEA, and pH value was adjusted to 3.0 by diluent ammonia. The flow rate was 0.6 mL . min(-1). Five mixed organotin compounds in a mix standard solution from 100 to 0.5 mu g . L-1 were applied for the method assessment. The experimental results indicate that the correlation coefficient of calibration curves (R-2) for each organotin compound was over 0.998 and the detection limits of the five organotin compounds were lower than 3 ng . L-1. Different mixed organic solvents including dichloromethane or toluene were used for extraction of organotin and the extraction condition of organotin from seawater was optimized. The 100 mL seawater acidized by hydrochloric acid was extracted by 10 mL carbon dichloride (CH2Cl2) with 2% tropolone for 10 min twice. Extracted organic solvents were mixed And blown to one drop by nitrogen with the rate of 1.7 mL . min(-1), then 1 mL acetonitrile was added to the drop for redissolving the organotin compounds. Finally, the mixed redissolution was filtered by 0.22 mu m organic filter membrane before analysis. it was found that the only organotin compound in seawater was triphenyltin (TPHT) and the content was 53.2 ng . L-1. The recoveries test from the standard addition for diphenyltin (DPHT), dibutyltin (DBT), tributyltin (TBT) and triphenyltin (TPHT) were over 80%. However, the recovery for trimethyltin (TMT) was relatively low and the value was 50%. The reason might be attributed to the decomposition or adsorption of those compounds during the extraction procedure. Further study on this subject is in progress.

Speciation Analysis of Organotin Compounds in Shellfish by Hyphenated Technique of High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

The hyphenated technique of high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry(HPLC-ICP-MS) was applied to the simultaneous determination of five organotin compounds in the shellfish samples. Agilent TC-C-18 column was selected, mobile phase of the HPLC was CH3CN:H2O: CH3COOH = 65:23:12 (V/V), 0. 05% TEA, pH = 3.0 at flow rate 0.4 mL/min. Five mixed organotin standards from 100 mu g/L to 0. 5 mu g/L was used for the method evaluation. The experimental results indicate that the linearity (R-2) for each compound was over 0.998. The shellfish samples were treated by supersonic extraction with mobile phase for 30min. Four organotin compounds including dibutyltin (DBT), tributyltin (TBT), diphenyltin (DphT) and triphenyltin (TPhT) in shellfish samples were detected with method mentioned above. It was found that the domain compounds in the samples were tributyltin (TBT) and triphenyltin (TPhT). The recoveries test from the standard addition for trimethyltin (TMT tributyltin (TBT), and triphenyltin (TPhT) were, over 80%. However, the recoveries for diphenyltin (DPhT) and dibutyltin (DBT) were relatively low, 37.3% and 75.2% respectively. The reason might be attributed to the decomposition of those compounds during the extraction procedure. The further study on this subject is under the progress.

氮杂多环光致发光分子用于食品中脂肪胺的分析及质谱鉴定

对含氮类光致发光分子2-（11H-苯[a]咔唑）-异丙基氯甲酸酯进行柱前衍生处理，并经荧光检测对脂肪胺进行高效液相色谱（HPLC）分离和质谱定性。衍生物于λ_(ex)=279nm产生强烈荧光，发射波长为λ_(ex)=380nm。40℃下在pH9．0的硼酸缓冲液中，衍生反应3min后获得稳定的荧光产物。在Eclipse XDB-C_8色谱柱（4．6mm×150mm，5μm）上，采用梯度洗脱对12种脂肪胺衍生物进行了优化分离。采用大气压化学电离源（APCI Source）正离子模式进行质谱定性，实现了各种脂肪胺衍生物的快速、准确测定。该方法具有良好的重复性，多数脂肪胺的线性回归系数大于0．9994，检出限在2．73～23．16fmol水平。

2-(11H-苯[a]咔唑)-乙酸在脂肪胺的高效液相色谱分离及质谱鉴定中的应用

采用新型荧光衍生试剂2-(11H-苯[a]咔唑)-乙酸(BCA)进行柱前衍生并经荧光检测对脂肪胺进行高效液相色谱(HPLC)分离和质谱定性。衍生物荧光激发和发射波长为λ_(ex)=285 nm,λ_(em)=384 nm。60℃下在乙腈溶剂中用N-乙基-N-[′(3-二甲氨基)丙基]碳二亚胺盐酸盐(EDC)作催化剂,衍生反应15 min后获得稳定的荧光产物。在Hypersil BDS C_(18)(4.0 mm×200 mm,10μm)色谱柱上,采用梯度洗脱对12种脂肪胺衍生物进行了优化分离。采用大气压化学电离源(APCI Source)正离子模式进行质谱定性,实现了各种脂肪胺衍生物的快速、准确测定。脂肪胺的线性回归系数不小于0.999 8,检出限(S/N=3)为5.73～31.3 fmol。

慢肝解郁胶囊质量标准的研究

目的：建立慢肝解郁胶囊质量标准。方法：采用TLC法鉴别方中丹参、当归、白芍、延胡索；用HPLC法测定白芍中芍药苷的含量。结果：在TLC色谱中可检出丹参、当归、白芍、延胡索的特征斑点；芍药苷在0．0982μg-0．4910μg范围内呈线性关系，r=0．9999（n=5），平均加样回收率为98．5％，RSD=0．5％。结论：所建鉴别方法专属性强，定量方法简便、准确，能有效地控制该制剂的质量。

圆萼刺参中的芦丁,熊果酸和齐墩果酸的定性定量分析

采用薄层色谱法(TLC)和反相高效液相色谱法(RP-HPLC)对藏药材圆萼刺参中的芦丁,熊果酸和齐墩果酸进行定性和定量的分析.定性分析:TLC法检定芦丁和熊果酸和齐墩果酸成分,薄层色谱条件是以V(乙酸乙酯)∶V(丁酮)∶V(甲酸)∶V(水)=10∶6∶1∶2为展开剂,喷以10 g/L.NaNO_2的1%甲醇溶液在105℃检定芦丁,以V(CHCl3)∶V(乙酸乙酯)=1∶1为展开剂,喷以V(H2SO4)∶V(甲醇)=1∶2溶液在105℃检定熊果酸和齐墩果酸.定量分析:RP-HPLC法测定圆萼刺参中芦丁,流动相:V(甲醇)∶V(0.4%H_3PO_4溶液)=38∶62;检测波长340 nm;RP-HPLC法测定熊果酸和齐墩果酸,流动相:V(甲醇)∶V(0.2%H_3PO_4)溶液=85∶15;检测波长215 nm;圆萼刺参中的齐墩果酸,在本种植物中首次发现.

液相色谱/质谱大气压化学电离源鉴定深海鱼油中长链不饱和脂肪酸

以1,2-苯并-3,4-二氢咔唑-9-乙基苯磺酸酯为衍生化试剂,在充氮的气氛下对鱼油进行皂化处理,所得皂化产物经正己烷萃取处理后进行柱前衍生化,再以HPLC/MS分离和鉴定。通过对长链脂肪酸分子的标记处理,其衍生物分子在质谱分析中呈现出双键位置的规范信息。通过建立模型计算式,借助不饱和脂肪酸的分子离子峰和特征碎片离子峰的质量数,计算不饱和的碳碳双键位置。共鉴定出23种脂肪酸。结果表明深海鱼油主要由C12-C22的脂肪酸组成,多不饱和脂肪酸含量占67.08%（峰面积百分比,下同）,其中C16∶19-十六碳烯酸（11.7%）;C16∶44,7,10,13-十六碳四烯酸（2.91%）;C18∶112-十八碳烯酸（11.1%）;C18∶46,9,12,15-十八碳四烯酸（3.62%）;C20∶113-二十碳烯酸（1.21%）;C20∶55,8,11,14,17-二十碳五烯酸（16.71%）;C22∶62,5,8,11,14,17-二十二碳六烯酸（10.53%）。所建立的方法为不饱和脂肪酸碳链中双键位置的确定提供了新的技术手段。

柱前衍生-高效液相色谱分离测定及质谱鉴定脂肪胺

采用新型荧光衍生试剂2-(2-苯基-1-氢-菲[9,10-d]咪唑)-乙酸(PPIA)进行柱前衍生,经荧光检测实现了脂肪胺的高效液相色谱(HPLC)分离测定及柱后质谱鉴定.60℃下在乙腈溶剂中用N-乙基-N′-[ (3-二甲氨基) 丙基 ]碳二亚胺盐酸盐(EDC)做缩合剂,衍生反应15 min可获得稳定的荧光产物.脂肪胺衍生物荧光检测波长为380 nm(激发波长为260 nm).在Eclipse XDB-C8 色谱柱上,采用梯度洗脱对12种脂肪胺衍生物进行了优化分离,测定了造纸厂废水、大鼠端脑和酸奶中脂肪胺的含量.经柱后在线质谱大气压化学电离源(APCI Source)正离子模式实现了各种脂肪胺衍生物的质谱鉴定,借助对活性中间体的质谱解析确定了衍生反应的反应机理.该方法具有良好的重现性和回收率,多数脂肪胺的线性回归系数大于0.9996;检出限为3.1～18 fmol (S/N＝3∶ 1)

安睡伴侣软胶囊中丁香酚含量测定方法研究

安睡伴侣软胶囊由纯天然传统藏药(包括丁香、肉豆蔻、胡椒、阿魏等6味药材)组方，经超临界CO2萃取其中的挥发油等活性成分后精制而成，具有安神、催眠、抗惊厥等保健功效，无毒副作用。丁香酚是安睡伴侣软胶囊中稳定的、有代表性的功效成分，目前测定药材药品中丁香酚含量的方法主要有液相色谱法(HPLC)和气相色谱法(GC)等。本试验建立了安睡伴侣软胶囊中丁香酚含量的气相色谱和液相色谱测定方法，采用这2种方法测试了5个批次的安睡伴侣软胶囊样品，并将2种方法的测定结果进行了对比。经数据统计分析(配对t检验)显示，HPLC法和GC法所得结果没有显著性差异，2种方法均可满足常规检验要求，都可以作为本制剂的质量检验方法。

四川西北地区川西獐牙菜指纹图谱研究（Ⅰ）

目的：建立川西獐牙菜药材甲醇溶解部分的HPLC指纹图谱。方法：反相高效液相色谱法，流动相甲醇．水(水中含0．02％的磷酸)，梯度洗脱，流速1．0mL·min^-1，检测波长260m，柱温30℃。结果：精密度、重复性、稳定性试验中共有峰峰面积、保留时间的RSD均小于5．0％；不同产地川西獐牙菜的相似度大于0．805。结论：该方法简便、实用、可靠，可作为川西獐牙菜药材的质量标准。

高效液相色谱／质谱分析抱茎獐牙菜提取物中的苷性成分

采用高效液相色谱／质谱法（HPLC／MS）分析抱茎獐牙菜提取物中5种苷性成分。在C18柱上，以甲醇（A：含20％水）和水（B：含10％甲醇）为流动相，流速1mL／min，线性梯度洗脱B从100％到0％，35min，液相色谱-质谱质联用（LC／MS），大气压化学电离源（APCI），对其中5种苷性成分进行定性鉴定。经HPLC／APCIMS分析确证，抱茎獐牙菜提取物中含有獐牙菜苦苷（swertiamarin）、龙胆苦苷（gentiopicroside）、獐牙菜苷（sweroside）、异红草苷（isoorientin）和獐牙菜山酮苷（swertianolin）。采用外标法定量，回收率分别为98．3％、106．7％、92．3％、88．2％和107．3％，该方法简便、快速、准确。

9种“藏茵陈”原植物中的7种有效化学成分研究

目的 研究藏药市场上9种“藏茵陈”植物中有效化学成分，根据所含成分的差异及其生理活性，确定这些植物的药用价值。方法 采用HPLC法测定7种成分的量。结果 9种植物的有效成分差异很大。结论 针对不同的化学成分用途，选择不同的植物，有效利用资源。[著者文摘]

Comparative Study of Contents of Four Tropane Alkaloids in Cultural and Wild Anisodus tanguticus

To assess the medicinal value of cultural Anisodus tanguticus,the contents of four bioactive tropane alkaloids,anisodine,anisodamine,scopolamine and atropine,in cultural and wild materials were determined by the HPLC method.The results showed that content of each alkaloid in the aboveground parts of cultural and wild samples was lower than that in roots,and this explained why it was not the whole plant but the root that was used as medicinal materials.The content of each alkaloid in the roots of one-year cultural material was lower than that in the two-year plants.The discrepancy of the total of four alkaloids between one-year and wild plants is not significant.Moreover,the total of four alkaloids,and the contents of anisodine,scopolamine,and atropine in two-year plants were higher than those in wild plant.Thus there is medicinal value in the cultivated A.tanguticus as well as wild A.tanguticus,especially in the two-year cultural A.tanguticus.

栽培花锚中抗肝炎活性成分的含量在不同生长期变化的研究

研究了花锚中去甲氧基花锚甙和花锚甙的含量随着不同生长期的变化趋势,为药材的合理栽培和采收提供科学依据.RP-HPLC法,使用VP-ODS C18柱,流动相为乙腈∶磷酸∶水(1‰),梯度洗脱程序:0～5.00 min乙腈的体积分数(以下同)为15%、5.01～14.00 min由15%增至25%、14.01～30.00 min由25%增至40%,流速为1 mL/min,柱温25℃,检测波长:254 nm.花锚甙和去甲氧基花锚甙、在花锚全草中的含量在不同生长期有明显变化.