柱前衍生液相色谱测定儿童食品中甜蜜素

在强酸条件下,样品中甜蜜素经次氯酸钠溶液处理后生成环己酰胺衍生物,在波长314nm处有强烈吸收,可直接用紫外检测器测定,建立柱前衍生液相色谱测定儿童食品中甜蜜素的方法。检出限为0.010mg/L,相关系数r=0.9996,样品测定回收率为95.0%-105.0%,相对标准偏差小于3.1%。本法简单、快速,灵敏度高,样品分析取得满意结果。     

超高效液相色谱-质谱法测定人体血浆中的环磷酰胺

建立了测定人体血浆中环磷酰胺血药浓度的超高效液相色谱-串联质谱方法.样品经甲醇沉淀蛋白,高速离心分离提取,用Waters Acquity UPLC BEH C18色谱柱(50mm×2.1mm,1.7μm)分离,以0.1％甲酸水溶液∶乙腈=(80∶20)为流动相进行洗脱,流速0.4mL·min-1,采用电喷雾质谱正离子模...     

柱前衍生-反相高效液相色谱法快速测定食品中的甜蜜素

样品溶于水,在酸性条件下,以次氯酸钠柱前衍生。在C18柱上用乙腈:水(体积比为70:30)为流动相,在314nm处测定,外标法反相高效液相色谱法快速测定食品中的甜蜜素,加标回收率为96.1%-101.8%之间,食品中共存的苯甲酸、山梨酸、安赛蜜、色素等不影响测定,方法简捷、准确。     

高效液相色谱-串联质谱法测定动物血浆中罗匹尼罗的浓度

建立高效液相色谱-串联质谱(LC-MS/MS)测定动物血浆中罗匹尼罗浓度的方法。血浆经乙酸乙酯萃取后,以HPLC分离,电喷雾离子化(ESI~+)串联质谱检测。以甲醇-乙腈-0.1‰冰醋酸(36:9:55)为流动相,流速为0.2mL·min~(-1),采用Ultimate XB-C 18柱(150mm×2.1mm,3μm)分离,在三级四极杆串联质谱中经电喷雾电离源(ESI)离子化,以多反应监测(MRM)方式进行检测。盐酸罗匹尼罗、盐酸苯海拉明(内标)的扫描离子对m/Z分别为261→114和m/Z 256→167。LC-MS/MS测定血浆中罗匹尼罗线性范围为0.02—400ng·mL~(-1),范围内线性关系良好(r=0.9998);以3个浓度水平的质量控制样品求得各浓度水平日内、日间精密度(RSD)均小于15.2%。在非临床药代动力学研究中,应用此法测定了受试兔子血浆中罗匹尼罗的浓度。该法灵敏、快速、准确,操作简便,样品处理方便,线性范围宽,该方法检测快速、专一、灵敏,可满足罗匹尼罗临床前药代动力学研究和临床药动学研究的要求。     

山海棠中β-胡萝卜素含量的反相高效液相色谱测定

反相高效液相色谱测定山海棠中β-胡萝卜素 ,方法快速、便捷 ,平均回收率在 (10 1.1± 1.10 ) % ,结果满意     

反相高效液相色谱法测定苦丁茶中的熊果酸

建立反相高效液相色谱法测定苦丁茶中熊果酸的新方法。乙醇回流提取 ,酸碱沉淀分离制备样品溶液 ,在以甲醇 -水 -磷酸二氢钠 -二乙胺 (90∶ 10∶ 0 .10∶ 0 .0 2 )为流动相、hypersil- C18柱、检测波长 2 2 0 nm、流速为 0 .6 m L/min的条件下 ,熊果酸与其他三萜成分在 2 0 min内达到基线分离。熊果酸在 0 .16 0 8—0 .80 4 0 mg/m L范围内 ,浓度与峰面积呈良好的线性关系 ,加标回收率为 98.0 6 %— 10 1.8% ,RSD=1.73%— 2 .16 %。该法适用于苦丁茶药材及其他制剂中熊果酸的质量分析检验 ,为天然植物中熊果酸的开发提供了简便、准确的测定方法。     

反相高效液相色谱法测定口香糖中的抗氧化剂BHA

采用 Zorbax XDB- C18柱 (4 .6× 15 0 mm) ,以乙腈和水按 6 0∶ 4 0的配比作流动相 ,流量为 1m L /min,柱温 30℃ ,检测波长 2 80 nm,建立了一种用反相高效液相色谱测定口香糖中 BHA的方法。检出限为0 .15 mg/kg,回收率在 83%— 10 1%之间 ,相对标准偏差小于等于 7.5 %。本法具有操作简便 ,灵敏、准确 ,重现性好等优点。适用于口香糖中 BHA的定量分析。     

高效液相色谱-紫外检测法测定食品中的过氧化氢

通过在60℃下超声提取,用亚铁氰化钾和乙酸锌沉淀蛋白质,通过0.45μm滤膜净化样品。利用水和乙腈在200nm波长紫外吸收弱的特点,降低基线噪音。在0.5mL/min流速下,色谱柱对过氧化氢的保留增大,可以与杂质较好分离。用反相高效液相色谱-紫外检测色谱法,在C18柱上不经过衍生化测定了食品中过氧化氢的残留。过氧化氢的检出限为1.5×10^-7mol/L。对实际样品进行检测时,平均回收率R≥75%,RSD≤3%。     

反相高效液相色谱荧光检测法测定新型咀嚼胶片剂中右美沙芬的血浆浓度

建立反相高效液相色谱荧光检测法测定口服新型咀嚼胶片剂后血浆中右美沙芬浓度的方法。采用Hanbon C18（4.6mm×250mm,5μm）色谱柱,以乙腈-水-磷酸-三乙胺（35∶65∶0.14∶0.10,V/V/V/V）为流动相,在流速0.6mL.min-1,进样量50μL,柱温30℃,荧光激发波长（Ex）和发射波长（Em）分别为280nm和320nm条件下,测定咀嚼胶片剂中右美沙芬的兔血药浓度。药物与杂质分离效果良好、线性范围为1—1000ng.mL-1,相关系数为0.9996。方法回收率和提取回收率分别为110.0%和83.9%。当S/N=3时,右美沙芬最低检出浓度可达1ng.mL-1。本方法准确、灵敏,可满足血药浓度检测和研究药代动力学行为的需要。     

高效液相色谱-质谱联用法测定饮料中的苯甲酸含量

建立了高效液相色谱-质谱联用法检测饮料中的苯甲酸.选用ZORBAX XDB-C18柱(50mm×2.1mm,3.5μm)为分析柱,流动相为乙腈-水,梯度洗脱,流速为200μL·min-1;质谱条件选用气动辅助电喷雾离子源(ESI),检测方式为负离子多离子反应检测(MRM);苯甲酸校准曲线线性范围为1-500μg/L;方...     

柱前衍生化RP-HPLC拆分盐酸洛美沙星对映异构体

以2,3,4,6-乙酰基-β-D-吡喃葡萄糖基异硫氰酸酯(GITC)为柱前衍生化试剂,建立了盐酸洛美沙星对映体柱前衍生化RP-HPLC拆分方法。采用了C18(4.6×250mm,5μm,Bnentnach)为色谱柱,在流动相为甲醇∶(3mmol.L-1四丁基溴化铵水溶液∶5mmol.L-1Na2HPO4的水溶液=1∶2)=25∶75,流速为1mL·min-1,检测波长284nm的色谱条件下,盐酸洛美沙星的非对映体在1.0—27.5μg.mL-1的浓度范围内有良好的线性关系,日内、日间精密度都3%,且获得了基线分离。该种方法能用于盐酸洛美沙星的手性拆分,也为盐酸洛美沙星的光学异构体的测定提供了参考。     

柱后衍生高效液相色谱法测定酱油、醋中黄曲霉素B1的含量

采用免疫亲和柱提取样品中的黄曲霉素B1,柱后衍生系统和高效液相色谱相结合,快速、准确地检测酱油、醋中的黄曲霉素B1的含量,检出限量可达2.5ppb.方法简便、灵敏度高,可作为常规手段推广应用.     

LC-MS法测定大鼠血浆中的冬凌草甲素含量

建立大鼠血浆中冬凌草甲素的LC-MS测定方法.用C18柱（150mm×2.0mm,5μm）色谱柱,乙腈-水（V/V=50∶50）为流动相,乙酸乙酯作为萃取剂,HPLC/电喷雾离子源质谱检测（HPLC/ESI-MS）.该方法测定乙酸乙酯萃取的冬凌草甲素在0.018-9.2μg·mL^-1浓度范围内线性关系良好（R2=0.9992）.定量下限为0.018μg·mL^-1,提取回收率和RSD分别为100.56％-101.74％和8.88％.采用LC-MS法检测乙酸乙酯萃取的大鼠血浆中的冬凌草甲素,可为进一步深入研究冬凌草甲素在人体内药代动力学特征提供可靠检测手段.     

Spectrofluorimetric Determination of Aliskiren in Tablets and Spiked Human Plasma through Derivatization with Dansyl Chloride

A simple and sensitive method has been developed and validated for the determination of aliskiren (ALS) in its dosage forms and spiked plasma. The method was based on the reaction of the drug with dansyl chloride in the presence of bicarbonate solution of pH 10.5 to give a highly fluorescent derivative which was measured at 501 nm with excitition at 378 nm in dichloromethane. Different experimental parameters affecting the development of the method and stability were carefully studied and optimized. The calibration curves were linear over the concentration ranges of 100–700 and 50–150 ng/mL for standard solution and plasma, respectively. The limits of detection were 27.52 ng/mL in standard solution, 4.91 ng/mL in plasma. The developed method was successfully applied to the analysis the drug in the commercial tablets and spiked plasma samples. The mean recovery of ALS from tablets and plasma was 100.10 and 97.81%, respectively. A proposal of the reaction pathway was presented.     

HPLC法测定大鼠盲肠内容物中5-氨基水杨酸的含量

建立高效液相色谱法测定5-氨基水杨酸在大鼠盲肠内容物中的含量.色谱柱为依利特C18柱（Hypersil BDS,200mm×4.6mm,5μm）,流动相为磷酸盐缓冲液（含0.01mol·L^-1四丁基溴化铵,pH 6.6）∶甲醇=75∶25 （V/V）,流速1.0mL·min-1,检测波长240nm.实验结果表明大鼠盲肠内容物中的内源性物质不干扰测定;线性范围为1.0-64.0μg·mL^-1（r=0.9994）;样品日内日间精密度的RSD均小于2％,回收率在99％-101％之间.本法快捷、灵敏、准确,可用于5-氨基水杨酸大鼠盲肠内容物药物浓度的测定.     

Spectrofluorimetric Determination of Oxamniquine in Dosage Forms and Spiked Human Plasma through Derivatization with 1-dimethylaminonaphthalene-5-sulphonyl chloride

A sensitive, simple and selective spectrofluorimetric method was developed for the determination of oxamniquine (OXM) in pharmaceutical formulations and biological fluids. The method is based on the reaction between the drug and 1-dimethylaminonaphthalene-5-sulphonyl chloride (dansyl chloride) in presence of 0.5 M sodium carbonate (pH 10) to yield a highly fluorescent derivative that is measured at 445 nm after excitation at 335 nm. The different experimental parameters affecting the development and stability of the reaction product were carefully studied and optimized. The fluorescence concentration plot was rectilinear over the range of 0.02–0.2 μg ml⁻¹ with a lower detection limit (LOD) of 0.007 μg ml⁻¹ and limit of quantitation (LOQ) of 0.02 μg ml⁻¹. The proposed method was successfully applied to the analysis of commercial capsules. The results obtained were in good agreement with those obtained using the official spectrophotometric method. Furthermore, the method was applied for the determination of oxamniquine in spiked human plasma, the mean % recovery (n = 4) is 97.77 ± 1.19. A proposal of the reaction pathway was presented.     

Spectrofluorimetric Determination of Fluvoxamine in Dosage Forms and Plasma Via Derivatization with 4-Chloro-7-Nitrobenzo-2-Oxa-1,3-Diazole

A highly sensitive and simple spectrofluorimetric method has been developed and validated for the determination of the antidepressant fluvoxamine (FXM) in its dosage forms and plasma. The method was based on nucleophilic substitution reaction of FXM with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole in an alkaline medium (pH 8) to form a highly fluorescent derivative that was measured at 535 nm after excitation at 470 nm. The factors affecting the reaction was carefully studied and optimized. The kinetics of the reaction was investigated, and the reaction mechanism was presented. Under the optimized conditions, linear relationship with good correlation coefficient (0.9995) was found between the fluorescence intensity and FXM concentration in the range of 65–800 ng ml⁻¹. The limits of detection and quantitation for the method were 21 and 64 ng ml⁻¹, respectively. The precision of the method was satisfactory; the values of relative standard deviations did not exceed 2.17%. The proposed method was successfully applied to the determination of FXM in its pharmaceutical tablets with good accuracy; the recovery values were 97.8–101.4 ± 1.08–2.75%. The results obtained by the proposed method were comparable with those obtained by the official method. The high sensitivity of the method allowed its successful application to the analysis of FXM in spiked human plasma. The proposed method is superior to the previously reported spectrofluorimetric method for determination of FXM in terms of its simplicity. The proposed method is practical and valuable for its routine application in quality control and clinical laboratories for analysis of FXM.     

三氟乙酸酐衍生化GC/MS/MS方法检验尿中吗啡

建立了人体尿中吗啡和O~6-单乙酰吗啡的衍生化GC/MS/MS定性、定量分析方法。以SKF_(525a)为内标,三氟乙酸酐为衍生化试剂,采用DB5-MS色谱柱对衍生化产物进行分析。尿中吗啡和O~6-单乙酰吗啡的质量浓度在0.05—10μg/mL范围内线性良好,线性相关系数r均为0.9901;方法回收率为65%—86%。检出限均为0.05ng/mL。该法操作简单,灵敏度高,适合作为法医毒物分析的常规方法。     

Determination of Ubiquinone in Blood by High-Performance Liquid Chromatography with Post-Column Fluorescence Derivatization Using 2-Cyanoacetamide

It was shown that ubiquinone (CoQ₁₀) and ubiquinol (CoQ₁₀H₂) produce fluorescence products under alkaline conditions when reacted with 2-cyanoacetamide. The reaction mixture from CoQ₁₀ gave fluorescence with excitation and emission maximum wavelengths at 442 nm and 549 nm, respectively. This reaction was considered to proceed via Craven’s reaction. Moreover, 2-cyanoacetamide was shown to be a useful reagent for high-performance liquid chromatography (HPLC) with post-column fluorescence derivatization of CoQ₁₀ and CoQ₁₀H₂ in blood. CoQ₁₀ showed a linear response in the range of 0.32–1276 ng, and the detection limit (S/N = 3) was 0.16 ng. Moreover, the sample pretreatment by deproteinization and extraction of CoQ₁₀ and CoQ₁₀H₂ from plasma using 1-propanol with potassium formate was effective for excellent separation of CoQ₁₀ and CoQ₁₀H₂ from other fluorescent substances in the blood. This simple and rapid pretreatment was considered to minimize the oxidation of CoQ₁₀H₂. On the other hand, CoQ₁₀ and CoQ₁₀H₂ in plasma samples obtained by finger prick were detected, as in venous blood obtained by venipuncture. Our method involving the simple and rapid collection of plasma by finger prick and sample pretreatment is thought to be applicable for the determination of CoQ₁₀H₂/total CoQ₁₀ ratio as a biomarker of oxidative stress.