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高效液相色谱法测定杜仲叶中的绿原酸 总被引:15,自引:0,他引:15
采用高效液相色谱法测定杜仲叶中绿原酸的含量。所用色谱柱为Shim-packCLC-ODS柱,以巯嘌呤为内标,以甲醇-0.01mol/L磷酸二氢钾缓冲液(体积比为25∶75;pH3.9)为流动相,UV检测波长为328nm。在上述色谱条件下,当绿原酸质量浓度为25~300mg/L时,以绿原酸对照品溶液与内标液的峰面积比为纵坐标(Y),绿原酸的质量浓度为横坐标(X),二者呈良好的线性关系,线性方程为Y=8.0368X+1.275×10-3,r=0.9999;平均回收率为99.89%,RSD=1.45%(n=6)。 相似文献
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建立了经鼻腔给药后人血浆中佐米曲普坦的液相色谱-质谱联用测定方法。血浆样品经乙酸乙酯-二氯甲烷(体积比4∶1)液-液提取后,以Hypersil BDS C6H5柱(4.6 mm×250 mm,5μm)为色谱柱,流动相为乙腈(含1%甲酸)-0.02 mol.L-1醋酸铵(体积比30∶70),流速为0.6 mL.m in-1,柱温:25℃,进样量:40μL,在Agilent 1100 LC/MSD XCT离子阱质谱仪上,以选择离子监测(SIM)方式进行定量分析,用于监测的离子为m/z288(佐米曲普坦)和m/z296(舒马普坦,内标物)。佐米曲普坦的定量下限为0.30μg.L-1,线性范围为0.30~25μg.L-1,方法回收率在82%~87%之间(n=5),精密度与准确度符合生物样品分析要求。该法操作简便、快速、灵敏度高,可用于佐米曲普坦临床血药浓度和药代动力学研究。 相似文献
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高效液相色谱法测定中药材补骨脂中补骨脂素和异补骨脂素的含量 总被引:6,自引:0,他引:6
建立了测定中药材补骨脂中补骨脂素和异补骨脂素含量的高效液相色谱法。采用的色谱条件为:Hypersil ODS色谱柱(150 mm×4.6 mm i.d., 5 μm),以乙腈-水(体积比为30∶70)为流动相,检测波长为245 nm。在此条件下,补骨脂素、异补骨脂素和内标物联苯苄唑获得了较好的分离。补骨脂素和异补骨脂素质量浓度分别为0.50~10.0 mg/L 时,组分与内标的峰面积比值与质量浓度之间的线性关系良好(r=1.000),最低检测限为10 μg/L (S/N=3) 。所建立的方法用于不同 相似文献
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建立了高效液相色谱法测定五星肠安中头孢唑啉钠和恩诺沙星的方法。采用Shim packCLC ODS柱(150mm×6mm,5μm),以乙腈 5g/L柠檬酸 三乙胺(体积比为160∶840∶2)为流动相,头孢唑啉和恩诺沙星在20~100μg/mL的范围内质量浓度与峰面积呈良好的线性关系,回归方程和相关系数分别为:A=31692 3ρ 4076 8,r=1 0000;A=108921ρ 21587 4,r=0 9999。头孢唑啉钠和恩诺沙星的平均回收率分别为99 9%、100 0%;RSD分别为0 70%、1 1%。方法可用于五星肠安的质量控制。 相似文献
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同位素内标稀释液相色谱-串联质谱法测定鱼贝类组织中残留的环丙氟哌酸 总被引:2,自引:0,他引:2
建立了不同鱼贝类肌肉组织中以氘代同位素为内标测定环丙氟哌酸残留量的液相色谱-串联质谱(LC-MS/MS)方法。样品加入内标环丙氟哌酸-D8和磷酸盐缓冲溶液(pH 7.0)后进行匀质并用乙腈超声提取,经正己烷脱脂后采用Waters Oasis MAX小柱净化,在Cloversil-C18柱上,以乙腈-0.05%三氟醋酸(体积比为25∶75)为流动相,采用多反应监测(MRM)模式,液相色谱-电喷雾质谱法测定。根据环丙氟哌酸和氘代内标物的定量离子质量色谱图的峰面积比值,采用内标法定量。结果表明,环丙氟哌酸和内标的定量离子峰面积比值与环丙氟哌酸浓度在0.1~50.0 μg/kg范围内呈现良好的线性关系,相关系数为0.9991,方法的定量检测限为0.1 μg/kg,回收率为92.5%~98.1%,相对标准偏差(RSD)小于4.3%。将该方法用于市场上10种鱼和贝类样品的检测,结果表明该法具有灵敏、准确的优点,完全满足残留分析的确证检测要求。 相似文献
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黄键王金娟周元元张敏王红卫王晓颖孙雪婷 《化学分析计量》2023,(6):34-39
建立同位素稀释-超高效液相色谱-串联质谱法同时测定化妆品中两种香兰素类香料的方法。取1 g样品,加入50μL质量浓度均为1 mg/L的香兰素-D3、乙基香兰素-D5混合同位素内标溶液,以甲醇为提取溶剂,溶解后定容至10 mL,在室温下超声提取15 min,离心分离后,取1 mL上清液用氮气吹干,再用1 mL 0.1%甲酸水溶液-甲醇(体积比为80∶20)定容,过滤后上机分析。经RRHD Eclipse Plus C18色谱柱分离后,使用ESI源对目标物进行电离,在多反应监测模式下绘制色谱图,内标法定量。在5~100μg/L范围内,香兰素、乙基香兰素与内标的质量浓度比与对应色谱峰面积的比线性关系良好,相关系数均大于0.999,方法检出限均为5μg/kg。空白样品加标回收率分别为87.8%~96.1%、80.1%~83.8%,测定结果的相对标准偏差分别为2.5%~3.8%、1.7%~4.6%(n=6)。该方法操作简便,可满足同时测定化妆品中两种香兰素类香料的要求。 相似文献
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建立小体积液液萃取-气相色谱-三重四极杆串联质谱法测定地下水中32种半挥发性有机污染物(SVOCs)的方法。采用2 mL二氯甲烷和正己烷混合溶剂(体积比为1∶1)加入到20 mL水样中,添加2 g NaCl,涡旋萃取60 s,经DB-5MS UI色谱柱(30 m×0.25 mm,0.25μm)分离,SRM模式检测,内标法定量。32种SVOCs的质量浓度在0.5~20μg/L范围内与色谱峰面积具有良好的线性关系,相关系数均大于0.995,方法检出限为0.002~0.06μg/L。样品加标回收率为72.5%~129%,测定结果的相对标准偏差为0.65%~21.1%(n=6)。该方法样品处理简单快捷,所需水样和有机试剂体积较少,能够满足地下水中32种SVOCs的高效测定。 相似文献
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超高效液相色谱-质谱/质谱联用法测定人血浆中的辛伐他汀 总被引:1,自引:0,他引:1
建立了超高效液相色谱-质谱/质谱联用法(UPLC-MS/MS)测定人血浆中辛伐他汀的浓度。血浆样品经乙醚-正己烷-异丙醇(体积比为80∶20∶3)提取,以洛伐他汀为内标,采用ACQUITY UPLCTM BEH C18柱(50 mm×2.1 mm,1.7 μm)分离,以乙腈-10 mmol/L乙酸铵水溶液(体积比为85∶15)为流动相,流速为0.25 mL/min,通过电喷雾离子化,采用多反应监测(MRM)方式进行正离子检测。线性范围为0.051~20.4 ng/mL,日内及日间测定的相对标准偏差不高于10%,平均回收率为91.6%。方法灵敏度高,分析速度快,操作简便,适用于辛伐他汀药物动力学和生物等效性研究。 相似文献
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Rahul P. Dixit Chandrashekhar R. Barhate Mangal S. Nagarsenker 《Chromatographia》2008,67(1-2):101-107
Simvastatin and ezetimibe are used to treat hyperlipidemia. A simple, selective and stability-indicating HPTLC method has
been established for analysis of simvastatin and ezetimibe. The method has been validated so that both drugs can routinely
be analyzed simultaneously. The method uses aluminum-backed silica gel 60F254 TLC plates as stationary phase with n-hexane–acetone 6:4 (v/v) as mobile phase. Densitometric analysis of both drugs was carried out in absorbance mode at 234 nm. This system was found
to give compact bands for simvastatin and ezetimibe (R
F 0.39 ± 0.05 and 0.50 ± 0.05, respectively). Linear relationships were obtained between response and amount of drug in the
range 200–1,600 ng per band with high correlation coefficients (r
2 = 0.9917 ± 0.0018 for simvastatin and r
2 = 0.9927 ± 0.0021 for ezetimibe). The method was validated for precision, robustness, and recovery. The limits of detection
and quantitation were 25 and 150 ng per band, respectively. Simvastatin and ezetimibe were subjected degradation by acid,
pH 6.8 phosphate buffer, oxidation, dry heat, and wet heat. The degradation products were well resolved from the pure drug
with significantly different R
F values. Because the method could effectively separate the drug from its degradation products, it can be used for stability-indicating
analysis. 相似文献
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Tao Mao Bo Hao Jin He Weilin Li Shengqing Li Ziniu Yu 《Journal of separation science》2009,32(17):3029-3033
A fast and novel sample preparation procedure: ultrasound assisted ionic liquid (IL) dispersive liquid extraction for the concentration of lovastatin and simvastatin in aqueous samples was developed. An IL ([C6MIM][PF6]) was used as the extraction solvent, and the factors affecting the extraction efficiency such as initial temperature, the volume of IL, pH of water samples, cooling time, and salt concentration were optimized. In combination with HPLC‐UV, both lovastatin and simvastatin exhibited a good linear range of 1–100 ng/mL. The limits of detection (LODs) of lovastatin and simvastatin were 0.17 and 0.29 ng/mL, respectively. Precisions of the proposed method (RSDs, n = 9) were 4.12 and 4.52%, respectively. This method has been successfully applied for the analysis of target compounds in three real water samples and good spiking recoveries were obtained in the range of 90.0–102.2% for lovastatin and 80.5–112.0% for simvastatin. These results indicated that ultrasound assisted IL dispersive liquid phase extraction would have good application prospect in the pretreatment of environmental samples. 相似文献
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气相色谱-电子捕获法测定血浆中的雷公藤甲素 总被引:6,自引:0,他引:6
血浆样品经碱化后用乙醚 氯仿 (体积比为 3∶1)混合液提取 ,浓缩的提取物与三氟醋酐进行衍生化反应 ,用气相色谱法分离、63Ni电子捕获检测器测定雷公藤甲素的含量。色谱柱为SE 5 430m× 0 2 5mmi d 交联石英毛细管柱。雷公藤甲素的质量浓度在 1 0 μg/L~ 5 0 0 μg/L范围内与峰面积线性关系良好 (r =0 9990 ) ,在血浆中的平均回收率为 96 3% ,最小检测限为 0 5 μg/L。方法重现性好 ,准确、灵敏 ,无杂质干扰 ,数据准确可靠 ,可用于临床生物样品中雷公藤甲素含量的测定。 相似文献
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Laxminarayana Burugula Ramesh Mullangi Nageswara Rao Pilli Ajitha Makula Durga Srinivas Lodagala Rajnarayana Kandhagatla 《Biomedical chromatography : BMC》2013,27(1):80-87
A simple, rapid and sensitive liquid chromatography–tandem mass spectrometric (LC‐MS/MS) assay method has been developed and validated for simultaneous quantification of sitagliptin and simvastatin in human plasma. Carbamazepine was used as an internal standard (IS). The analytes and IS were extracted from the human plasma by liquid–liquid extraction technique. The reconstituted samples were chromatographed on an Alltima HP C18 column using an isocratic solvent mixture [acetonitrile–5 mm ammonium acetate (pH 4.5), 85:15 (v/v)] at a flow rate of 1.0 mL/min. Method validation was performed as per Food and Drug Administration guidelines and the results met the acceptance criteria. The calibration curves obtained were linear (r2 ≥ 0.99) over the concentration range of 0.10–501 and 0.05–105 ng/mL for sitagliptin and simvastatin, respectively. The results of the intra‐ and inter‐day precision and accuracy studies were well within the acceptable limits. Both the analytes were found to be stable in a battery of stability studies. The method is precise and sensitive enough for its intended purpose. A run time of 3.0 min for each sample made it possible to analyze more than 300 plasma samples per day. The developed assay was successfully applied to a pharmacokinetic study in human volunteers. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
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用线性扫描极谱法研究辛伐他汀的电化学行为。在pH 6.88的0.12mol·L-1磷酸氢二钠-磷酸二氢钾缓冲溶液中,辛伐他汀于-1.188V(vs.SCE)处产生一灵敏的吸附波,其一次微分线性扫描峰电流与辛伐他汀质量浓度在0.01~5.0mg·L-1范围内呈线性关系,检出限(3S/N)为7.0μg·L-1。对5.0mg·L-1辛伐他汀溶液进行6次平行试验,相对标准偏差(n=6)为0.53%,方法可用于测定其片剂中辛伐他汀含量。 相似文献
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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
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Victoria F. Samanidou Dimitrios E. Giannakis Antonia Papadaki 《Journal of separation science》2009,32(9):1302-1311
Herein a quantitative method for the determination of seven penicillins in bovine plasma and veterinary drugs has been developed. Amoxicillin (AMO), ampicillin (AMP), penicillin G (PENG), penicillin V (PENV), oxacillin (OXA), cloxacillin (CLO) and dicloxacillin (DICLO) were separated on a Perfectsil ODS‐2 (250×4 mm, 5 μm) column, using gradient elution, with a mobile phase of 0.1% v/v TFA and ACN–methanol (90:10 v/v). PDA detection was used at 240 nm. Penicillins were isolated from bovine plasma by SPE on Lichrolut RP‐18 cartridges with mean recoveries from 85.7 to 113.5%. Colchicine (3 ng/μL) was used as an internal standard. The developed method was validated in terms of selectivity, linearity, accuracy, precision, stability and sensitivity. Repeatability (n = 5) and between‐day precision (n = 5) revealed RSD < 12%. The detection limits in the bovine plasma were estimated as 18 ng for AMO and AMP, 25 for PENG, PENV and OXA, 3 ng for CLO and 12 ng for DICLO. Spiked plasma samples were stable for 1 wk, except for AMP and CLO, which were stable for 3 wk and OXA for 4 wk. AMO, PENG and PENV were stable for two freeze–thaw cycles, OXA, CLO and DICLO for four, while AMP only for one. 相似文献