共查询到20条相似文献,搜索用时 9 毫秒
1.
《Analytical letters》2012,45(4):281-290
Abstract A highly sensitive method for the determination of meperidine and normeperidine in biological fluids is presented. Concentrations as low as 5 ng meperidine and 25 ng normeperidine per ml of sample can be determined. The recovery of meperidine from control plasma and urine was 91.3 to 102.5% and the recovery of normeperidine was 64.7 to 82.8%. The method has been successfully used for the determination of meperidine in human plasma and urine and of normeperidine in human urine. 相似文献
2.
A gas chromatographic method was established for the quantitative analysis of pipemidic acid. The method is based on alkylation of pipemidic acid with diazomethane catalyzed by boron trifluoride. The sample was chromatographed on a stainless steel column packed with 5% OV-101 on Chromosorb G-HP and n-octacosane was used as an internal standard. Quantitation is achieved by measuring peak-height ratio. The method was satisfactorily applied to the analysis of pipemidic acid in tablet. 相似文献
3.
《Analytical letters》2012,45(11):845-856
Abstract An improved procedure for the GLC determination of acetaminophen (N-acetyl-p-aminophenol) in the presence of N-butyryl-p-aminophenol (internal standard) is described. The method is based on the extraction of acetaminophen from plasma with ethyl acetate containing a known amount of N-butyryl-p-aminophenol. Following a clean-up step with a basic buffer solution and neutralization with acid, both compounds are reextracted into ethyl acetate. The ethyl acetate is evaporated to dryness and the residue dissolved in 5 μl of pyridine and 15 μl of acetic anhydride at 42°C. One to 2 μl samples are injected directly into the gas chromatograph. This extraction process does not give rise to troublesome interfering peaks in the chromatogram. In addition, it prevents late-eluting peaks which inhibit efficient processing of samples. The recovery of acetaminophen is approximately 54%, and the limit of quantitation 0.5 μg/ml of plasma. Data are presented to illustrate the practicality of the method for bioavailability evaluation from acetaminophen plasma levels after oral administration of 325 mg of an acetaminophen dosage form. 相似文献
4.
《Analytical letters》2012,45(5-6):639-648
Abstract An improved procedure for the determination of caffeine in the presence of bupivicaine (internal standard) using gas liquid chromatography with nitrogen phosphorous detection is described. The method is based on the extraction of caffeine from plasma with a mixture of chloroform and isopropanol (95:5). The chloroform and isopropanol mixture is evaporated to dryness and the residue dissolved in 500 μl of ethyl acetate. One to 2 μl samples are injected directly into the gas chromatograph. This extraction process doesn't give rise to troublesome interfering peaks in the chromatogram. The recovery of caffeine from plasma and breast milk is approximately 99.7% and 94.1% respectively. The coefficient variation of the assay from plasma and breast milk is 2.90% and 1.18% respectively. The limit of quantitation is 0.05 mcg/ml of plasma or breast milk. Data are presented to illustrate the practicality of the method for bioavailability and pharmacokinetic evaluation of caffeine plasma and breast milk levels after oral administration of 100 mg of caffeine to lactating mothers. 相似文献
5.
6.
Simutaneous analysis of seven commonly used herbicides, 2,4-D methyl ester, 2,4-D methyl ester, 2,4,5-T methyl ester, silvex methyl ester, ramrod, CIPC and DEF, by gas-liquid chromatography with an electron capture detector was attempted. Two packed columns (which are generally used for the analysis of chlorinated pesticides) and two chemically bonded fused silica capillary columns were used for the analysis. When the packed columns were used, ramrod always interfered with the analysis of 2,4-D methyl ester and/or silvex methyl ester. Complete separation with reasonable analysis time can be achieved using one of the chemically bonded fused silica capillary columns. 相似文献
7.
The flow diagram of this on-line sample pretreatment system is shown in Fig. I. 相似文献
8.
固相萃取-高效液相色谱法测定人血浆中的川芎嗪 总被引:7,自引:0,他引:7
建立了高效液相色谱测定人血浆中川芎嗪浓度的方法。色谱条件:分析柱为Luna C18(150 mm×4.6 mm i.d.,5 μ
m),流动相为甲醇-乙腈-醋酸盐缓冲液(pH 5.0)(体积比为50∶8∶42),流速1.0 mL/min,柱温40 ℃,检测波长280 nm。
血浆样品预处理采用C8固相小柱萃取法。方法的线性范围为25~5000 μg/L,线性相关系数为0.9999。高、中、低浓度
的川芎嗪在标准血浆样品中的平均提取回收率为96.72%~100.90%,日内和日间相对标准偏差(RSD)小于8.64%,准确度
为99.59%~103.26%,检测限为10 μg/L。该方法的各项效能指标符合生物样品的分析要求,可用于川芎嗪制剂的人体药
代动力学研究。 相似文献
9.
10.
11.
高效液相色谱法测定人血浆中的辛伐他汀 总被引:3,自引:0,他引:3
建立了高效液相色谱法监测人口服辛伐他汀药物后的血药浓度。血样用环己烷-二氯甲烷(体积比为3.5∶1)提取,以洛伐他汀为内标,在237nm波长下检测;色谱柱:LichrospherC18(200mm×4.6mmi.d.,5μm),流动相:乙腈-水(体积比为70∶30);流速:1.2mL/min。血药浓度在0.25~50.0μg/L范围内与峰面积和内标峰面积的比值之间线性关系良好,日内及日间相对标准偏差(n=5)分别低于7.94%和8.58%,回收率高于93.3%。方法灵敏、准确、快速,适用于药物动力学和药效学研究。 相似文献
12.
13.
建立了胶束电动毛细管色谱同时分离测定阿咖酚散中咖啡因、对乙酰氨基酚、阿司匹林3种有效成分的方法。对以有机碱三乙醇胺为改进剂的胆酸胶束相进行了优化,对改进剂的影响机理进行了详细讨论。最佳电泳条件如下:以40 mmol/L硼酸盐-60 mmol/L胆酸-12.5%三乙醇胺(pH 12.0)为缓冲体系,分离电压为15 kV,检测波长为254 nm。在上述条件下,14 min内实现了阿咖酚散中3组分的基线分离。咖啡因、对乙酰氨基酚和阿司匹林的线性范围分别为18.75~900.0(r=0.999 9)、2.60~62.50(r=0.992 9)、79.17~3 800 mg/L(r=0.994 0)。上述3组分迁移时间和峰高的相对标准偏差分别不高于1.8%和6.8%。咖啡因、对乙酰氨基酚和阿司匹林的检出限分别为4.6、0.17、38 mg/L。应用该法测定阿咖酚散中上述3组分,加标回收率分别为100%、100%和102%,可满足实际样品分析要求。所建立的方法简便、快速、灵敏、经济,能同时进行阿咖酚散中多种成分的分离测定。 相似文献
14.
茶叶中咖啡因的超临界流体分析 总被引:6,自引:0,他引:6
用超临界流体法 (SFC)测定茶叶中的咖啡因 ,在二氧化碳流动相中加入体积分数为 5 %的甲醇后 ,得到了良好的分离效果。该方法具有样品前处理简单 ,共存组分不干扰测定 ,分析速度快等优点 ,可以用于茶叶中咖啡因的快速分析。 相似文献
15.
高效液相色谱法测定血浆中左亚叶酸钙的含量 总被引:2,自引:0,他引:2
建立了测定血浆中左亚叶酸钙含量的RPHPLC方法。采用DiamonsilC18色谱柱(150mm×4.6mm,5μm),乙腈50mmol/L磷酸氢二钾/磷酸二氢钾缓冲溶液(10∶90,V/V,用磷酸调pH至4.0)为流动相,用前经0.45μm的过滤膜,超声脱气,流速为1.0mL/min,紫外检测波长为290nm,柱温为35℃,进样量20μL。该方法最低检出限为0.2ng;线性范围为0.05~10mg/L,方法平均回收率在97.0%以上;日内及日间精密度的相对标准偏差分别小于4%和6%。该方法简单,快速,灵敏度高,重复性好。 相似文献
16.
反相高效液相法测定血浆及尿液中的异烟肼 总被引:5,自引:0,他引:5
建立了血浆及尿液中异烟肼的高效液相快速测定方法 ,以满足临床药物分析和法医学鉴定的需要 ,提高对血浆及尿液中异烟肼浓度检测的准确性。以香草醛为衍生化试剂 ,将异烟肼经柱前衍生为异烟肼 香草醛腙 ,直接对处理后样品中的腙进行定性、定量分析。以在空白人体液样本中定量添加标准异烟肼的方法考察了样品的前处理方法、仪器条件、线性范围、精密度、回收率等 ,并对健康受试者血液中的异烟肼浓度进行了监测。结果表明 ,方法的线性范围为 0 2mg/L~ 1 2 0mg/L ;检测限为 0 2mg/L ;日内、日间精度均小于 4 0 % (n =5) ;回收率在96 3 %以上。 相似文献
17.
高效液相色谱法测定人血浆中的芦氟沙星 总被引:2,自引:0,他引:2
建立了测定人血浆中芦氟沙星质量浓度的高效液相色谱法 ,血浆用二氯甲烷提取 3次 ,以 UltrasphereODS(4.6mm i.d.× 2 5 0 mm)为色谱柱 ,流动相为甲醇 -1 0 mmol/L 溴化四丁铵 -三乙胺 (体积比为 3 2∶ 68∶0 .5 ) ,用磷酸调 p H2 .8,检测波长 2 95 nm,流速为 1 .2 m L/min,以培氟沙星为内标。血浆中芦氟沙星的线性范围为 0 .1~ 1 0 mg/L ,最低检测质量浓度为 0 .0 5 mg/L ,回收率为 99.7% ,日内、日间 RSD分别为 2 .3 3 %和3 .83 %。方法简便、快速、准确 ,适用于人血浆中芦氟沙星质量浓度的测定。 相似文献
18.
An ion chromatography‐inductively coupled plasma mass spectrometric (IC‐ICP‐MS) method for the speciation of sulfur compounds, namely sulfite [SO32?], sulfate [SO42?] and thiosulfate [S2O32?], was described. Ionic sulfur compounds were well separated in about 3 min by ion chromatography with a Hamilton PRP‐X100 column as the stationary phase and 60 mmol L?1 NH4NO3 and 0.1% v/v formaldehyde (HCHO) solution (pH = 7) as the mobile phase. The analyses were carried out using dynamic reaction cell (DRC) ICP‐MS. The sulfur‐selective chromatogram was determined at m/z 48 as 32S16O+ by using its reaction with O2 in the reaction cell. The method avoided the effect of polyatomic isobaric interferences at m/z 32 caused by 16O16O+ and 14N18O+ on 32S+ by detecting 32S+ as the oxide ion 32S16O+ at m/z 48, which is less interfered. The detection limit of various species studied was in the range of 3.6–4.6 ng S mL?1. The accuracy of the method has been verified by comparing the sum of the concentrations of individual sulfur compounds obtained by the present procedure with the total concentration of sulfur in several natural water samples. The recovery was in the range of 97–102% for various compounds studied. 相似文献
19.
P. W. W. Kirk R. Perry J. N. Lester 《International journal of environmental analytical chemistry》2013,93(3-4):293-309
Abstract A comparison of gas-liquid chromatography, differential-pulse polarography and a colorimetric method for the determination of nitrilotriacetic acid in settled sewage, sewage effluent, potable water, soil extracted water and deionised water has been undertaken. Differential-pulse polarography has also been applied to the determination of nitrilotriacetic acid in saline samples. By statistical analysis of replicate determinations, accuracy and precision have been evaluated, and calibration linearity assessed. Interferences were observed for sewage samples when analysed by all three methods. Precision was generally higher for differential-pulse polarography down to 100 μgl?1, although only gas-liquid chromatography is applicable to concentrations below 25μgl?1 in non-saline samples. The colorimetric method was not applicable to concentrations below 500 μgl?1 of nitrilotriacetic acid. 相似文献