共查询到20条相似文献,搜索用时 46 毫秒
1.
孙芳 《理化检验(化学分册)》2001,37(5):228-228
50 %的卫生用倍硫磷乳油杀虫剂是具有触杀、胃毒和渗透作用的广谱杀虫剂 ,可用于防治苍蝇、蚊子、臭虫、跳蚤等多种害虫 ,其化学名称 :0 ,0 二甲基 0 4 (甲硫基苯基 3 甲基 )硫代磷酸酯 ,简称倍硫磷 ,化学结构式为沸点为 87℃ /1.333Pa ,相对密度为d2 04 =1.2 50 ,微溶于水 ,对光稳定。目前国内对倍硫磷含量的测定似尚无成熟的方法。本文以甲醇∶水 (8∶2 )为流动相 ,采用反相高效液相色谱法成功地测定倍硫磷的含量 ,其精密度高 ,回收率好。1 试验部分1.1 仪器与试剂日本岛津公司LC 10AD高效液相色谱仪 ,50型过滤器 ,注射式试… 相似文献
2.
报道了反相高效液相色谱法测定血浆中氢溴酸右美沙芬 ( DM)方法。采用Novapak C84μm,1 5 0 mm× 3.9mm i.d.分析柱 ,以乙腈∶水 =5 0∶ 5 0 ( V/V ,加0 .5 % HAc,三乙胺调节 p H至 4.3)为流动相 ,荧光检测器检测 ,DM的最小检出浓度为 0 .2 ng/m L。方法回收率为 93.71 % ,变异系数 3.5 3% ,操作简便 ,灵敏度高 ,适于血浆中 DM测定及药代动力学研究 相似文献
3.
4.
5.
建立了大鼠血浆中河豚毒素(TTX)反相离子对高效液相色谱测定方法。血浆样品加水涡漩,再加沉淀剂V(乙腈)∶V(含0.5%HAc的甲醇液)=3∶1),旋涡离心后取上清液进样测定。色谱柱为Agilent ZorbaxSB C18柱(150 mm×4.6 mm×5μm);流动相为10?N-90%的8 mmol/L庚烷磺酸钠与0.005%TFA混合溶液,配好后调到pH5.0;紫外检测波长196 nm;流速1.0 mL/min;柱温为室温。本方法TTX标准品检出限为1.055 mg/L,血浆中TTX的检出限为0.1055 mg/L。血浆中TTX的线性范围为21.1~211 mg/L,r=0.9989。日内和日间精密度RSD均小于3%。本方该法准确、专属性强,适用于血浆中TTX的浓度测定。 相似文献
6.
利用反相高效液相色谱(RP-HPLC)建立鳗鲡血浆中盐酸环丙沙星(CPFX)残留的测定方法.采用RP ODS色谱柱,以甲醇-四丁基溴化铵(30:70 v/v)为流动相,流速1 mL/min,进样量20μL,荧光激发波长(Ex)277 nm,荧光检测波长(Em)453 nm.鳗鲡血浆样品用二氯甲烷进行提取前处理,然后进行HPLC分离-荧光检测.盐酸环丙沙星溶液浓度在0.01~10.24 μg/mL范围与色谱峰高呈良好线性关系(r=0.9997),最低检测限为0.005μg/mL,标准添加平均回收率大于80%.方法灵敏简便,可用于鳗鲡体内盐酸环丙沙星残留的测定与药代动力学研究. 相似文献
7.
8.
反相高效液相色谱法测定血浆中的单硝酸异山梨酯 总被引:4,自引:0,他引:4
建立了反相高效液相色谱测定血浆中单硝酸异山梨酯浓度的方法。样品在碱性条件下经二氯甲烷提取后,用C18柱进行分离,以H2O(用0.03 mol/L氨水调pH至7.8)-乙腈(体积比为80∶20)为流动相,对乙酰氨基酚为内标,于230 nm处测定。结果表明,单硝酸异山梨酯的质量浓度为20~1000 μg/L时其峰面积与内标峰面积之比与单硝酸异山梨酯浓度有良好的线性关系。方法的最低检测质量浓度为12 μg/L,平均回收率为(97.11±2.45)%~(104.34±2.17)%,日内测定的相对标准偏差(RSD)≤2.52%,日间测定的RSD≤5.21%。 相似文献
9.
采用反相高效液相色谱法测定阿莫西林并对测定条件及有关参数进行了试验.用Shim-Pack VP-ODS柱作色谱柱,以磷酸盐缓冲液(pH 5.0)及乙醇以90比10的混合液为流动相,流速为1.0 mL·min-1,在228nm波长处测定阿莫西林的含量,其线性范围为0.045~0.60 g·L-1,相关系数为0.9974.将方法应用于阿莫西林胶囊的测定,测定结果的相对标准偏差值小于0.6%,用标准加入法作回收试验,回收率结果在94.7%~101.3%之间. 相似文献
10.
建立了反相高效液相色谱法测定饮料中苯甲醛的方法。当苯甲醛的质量浓度在1.0~100.0 mg·L-1范围时,苯甲醛的浓度与色谱峰面积呈线性关系,线性相关系数为0.999 8。苯甲醛的回收率为99.3%-102.6%,相对标准偏差为2.0%~3.4%,方法的检出限为0.1 mg·kg-1。 相似文献
11.
A rapid, sensitive and specific method based on high performance liquid chromatography-electrospray ionization-mass spectrometry was developed for the determination of tiopronin in human plasma. In this study, vitamin C and dithiothreitol were used as the reducer and to release and stabilize tiopronin from dimeric mixed forms with endogenous thiols encountered during pretreatment of plasma samples. The separation was successfully achieved on an Agilent SB-Aq column packed with 5 μm C18 silica, using an aqueous formic acid solution (pH 4.5–4.7), 0.5 mM tris(hydroxymethyl)aminomethane and methanol (95:5, v/v) as the mobile phase. Mass spectra were acquired in selective ion monitoring mode, using the [M ? H] ? ions of tiopronin at m/z 162.0 and the [M ? H]? of the internal standard sodium cyclamate at m/z 178.0, respectively. This quantitative assay was fully validated with respect to precision, repeatability and accuracy. The correlation coefficients were >0.9995 in the range 0.025–8.15 μg mL?1 in human plasma. The mean recoveries were above 85%. The limit of quantitation was 0.012 μg mL?1 with a relative standard deviation of inter-day and intra-day accuracy of less than 15%. This LC-ESI-MS method was also successfully applied to a pharmacokinetic study after oral administration of formulated tiopronin to healthy volunteers. The elimination half-life (T 1/2) was 21.5 ± 11.1 h. 相似文献
12.
Pidotimod, a synthetic dipeptid, has been shown to affect in a positive way some immune functions in humans. It induces an increase in the expression of interleukin-2-T-lymphocyte receptor and can play an important role as an immunostimulating agent, improving immunodefences. The speration and determination of pidotimod in plasma was achieved by using Zorbax Rx-Cl8 colunm. with a guard column. 相似文献
13.
Tao-Min Huang Chun-Hui Deng Ying-Jia Yu Xiao-Wei Zheng Geng-Li Duan 《Chromatographia》2006,63(11-12):551-556
An accurate, simple and sensitive method based on reversed-phase high-performance liquid chromatography with UV detection has been developed for determination of tiopronin (TP) in human plasma. TP in plasma was reacted with p-bromophenacyl bromide (p-BPB) to give the TP-p-BPB adduct and this derivative was then extracted from the plasma on a silica gel cartridge. Potential interfering compounds were removed by washing with water, and the TP-p-BPB adduct was then eluted with acetonitrile. The organic phase obtained was evaporated to complete dryness under a stream of nitrogen. The residue was dissolved in acetonitrile and this solution was injected on to a reversed-phase ODS HPLC column. The mobile phase was usually the ternary mixture acetonitrile–water–trifluoroacetic acid, 40:59.88:0.12 (v/v). The retention times of TP-p-BPB and the internal standard adduct were 14.4 and 17.9 min, respectively. No interfering peaks were encountered in several blank plasma samples examined. The limit of detection for TP was 12 ng mL?1. Extraction recovery exceeded 70%. The calibration plot for the TP derivative was linear in the range 40?4000 ng mL?1, regression coefficient 0.9989, and the coefficient of the variation of the points of the calibration plot was below 10%. The method was validated appropriately and successfully applied to the determination of TP in human plasma. 相似文献
14.
A sensitive liquid chromatographic–electrospray ionization–mass spectrometric (LC–MS) method has been developed for direct measurement of the concentration of tiopronin in human plasma. Hydrochloric acid solution was used to stabilize the tiopronin and prevent formation of a dimer, or reaction with endogenous thiols. The method involved liquid–liquid extraction of tiopronin from plasma samples with ethyl acetate, simple reversed-phase chromatography, and mass spectrometric detection with nanogram detection limits. Acetaminophen was used as internal standard (IS). The limit of quantification was 5 ng mL?1 (RSD 4.3%). The method was validated within the linear range 5–500 ng mL?1. The correlation coefficient for the calibration regression line was 0.9997 or better. Intra-day and inter-day accuracy were better than 15%. The method has been successfully used for a pharmacokinetic study with human subjects. Among the pharmacokinetic data obtained, t 1/2 was 2.37 ± 0.63 h and T max was 4 h. 相似文献
15.
提出了应用气相色谱-质谱法测定血浆中双氯芬酸钠含量。血浆样品中双氯芬酸钠经盐酸提取,并加入三甲基硅烷衍生化试剂进行衍生化,所得衍生化产物经萃取、净化后供气相色谱分离及质谱测定。采用选择离子质谱扫描方式,供试品双氯芬酸钠-三甲基硅烷衍生物定量选择离子检测质荷比为m/z367,内标物布洛芬-三甲基硅烷衍生物定量选择离子检测质荷比为m/z263。双氯芬酸钠的线性范围为0.005~5.0mg·mL-1,检出限(3S/N)为0.5μg.L-1。方法回收率在94.6%~97.4%之间,日内、日间相对标准偏差(n=6)均小于5%。 相似文献
16.
Jianming Huang Weiyu Weng Di Cao Xubing Huang Jian Wang Hao Yu 《Chromatographia》2005,62(9-10):471-474
A rapid and specific reversed-phase high performance liquid chromatography (RP-HPLC) method for the determination of palmatine in rabbit plasma has been developed and validated. The chromatographic separation was performed on a C18 column at 40 °C. The mobile phase, delivered at 1.0 mL min?1, consisted of acetonitrile/phosphate buffer (pH 3.0) 40:60 (v/v). The detection wavelength was set at 345 nm. Palmatine and internal standard (IS) berberine were extracted from plasma by solid-phase extraction using C18 cartridges. Linearity was confirmed in the concentration range of 0.01 to 5 μg mL?1, the inter-day and intra-day RSDs were within 10.0, the recoveries of palmatine ranged from 93.1 to 110.3, and the limit of detection (LOD, S/N > 3) was 0.002 μg mL?1. The method is applicable to the determination of palmatine in rabbit plasma after intravenous administration of palmatine. 相似文献
17.
《Analytical letters》2012,45(14):2200-2209
A new, sensitive RP-HPLC method was developed for the determination of oseltamivir phosphate in capsules and plasma. The method was based on the reaction of the drug with 4-chloro-7-nitrobenzofurazan in borate buffer solution of pH 8.50. Isocratic chromatography was performed on a C18 column with acetonitrile–10 mM nitric acid (pH 3, 60 + 40, v/v) as the mobile phase with fluorescence detection (λex: 470 nm, λem: 541 nm). Mexiletine hydrochloride was used as an internal standard. Analytical parameters were evaluated. The calibration range was linear from 50.0–750.0 ng/ml. The mean percentage recovery in capsules and plasma were 99.95% and 95.42%, respectively. 相似文献
18.
基于硫普罗宁[化学名为N-(2-巯基丙酰基)-甘氨酸]对铁(Ⅲ)的还原反应和还原后的铁(Ⅱ)与邻菲啰啉的显色反应生成吸收峰在508nm处的络合物,并应用了流动注射技术,提出了间接测定硫普罗宁的流动注射光度分析法。设计并自制了流动注射分析仪,采用光栅分光光度计作为检测单元,此仪器的测定频率达到85次.h-1。硫普罗宁的质量浓度在4.00~450mg.L-1范围内与吸光度呈线性关系,检出限(3s/k)为0.56mg.L-1。应用此方法分析了硫普罗宁片剂及针剂样品,所得测定值与标准方法的测定值相符。以此两种样品为基体,加入标准溶液作回收试验,测得片剂及注射剂的回收率分别为100.5%及99.2%。 相似文献
19.
A sensitive, simple, and accurate reversed-phase column liquid chromatographic (RP-LC) method with daidzein as an internal standard and UV detection at 348 nm has been developed for determination of linarin in beagle dog plasma. Plasma protein was precipitated by addition of acetonitrile and the remaining solution was evaporated to dryness. The resulting residue was then reconstituted in methanol and injected on to a 250 mm × 4.6 mm i.d., 5 μm particle, ODS analytical column. The mobile phase was a gradient prepared from acetonitrile and an aqueous solution (0.4%) of phosphoric acid; the flow rate was 1.0 mL min−1. Response was a linear function of concentration over the range 3.4–1,373.3 ng mL−1; the correlation coefficient (R
2) was 0.993. Mean recovery was 74.2%. Within-day and between-day precision were better than 8.8% relative standard deviation (RSD). The limit of quantification was 3.4 ng mL−1. This RP-LC method was used successfully in pharmacokinetic studies of linarin in beagle plasma after administration of Yejuhua injection. 相似文献