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1.
建立高效液相色谱法测定豆奶粉中三种异黄酮含量的测定方法。采用LC-20AT高效液相色谱系统,以甲醇-水（5.5：4.5）为流动相,检测波长为260 nm,流速为0.8 mL.min-1。待测组分与其他组分分离度良好,结果表明染料木苷、大豆黄素、染料木素线性范围分别为11.47～172μg.mL-1（r=0.9998）,5.33～80μg.mL-1（r=0.9999）,8.26～124μg.mL-1（r=0.9998）,平均回收率分别为98.9%,98.7%,99.4%,相对标准偏差分别为0.3%,1.8%,2.0%。该方法准确且重现性好,结果可为不同人群选择豆类食品提供科学依据。 相似文献
2.
本文用磺化四苯基卟啉（ＴＰＰＳ_４）作柱前衍生试剂,研究了试剂与Ｃｕ（Ⅱ）、Ｚｎ（Ⅱ）的络合反应．四乙基溴化铵为离子对试剂,离子对高效液相色谱－光度法是快速分离并测定铜、锌的新方法．在 ＯＤＳ色谱柱上,用乙腈－水（２２： ７８, ｖ／ｖ）作流动相,以双波长（４１５ｎｍ和４２５ｎｍ）进行光度检测．络合物在８ｍｍ内出峰完毕,检测下限为Ｃｕ０．０９（×１０~(－３)μｇ／ｍｌ）,Ｚｎ ０．０８（× １０~(－３)μｇ／ｍｌ）．将所建立的方法用于树叶中铜和锌的测定,结果令人满意． 相似文献
3.
建立了HPLC法测定小儿喜食浆中柚皮苷含量测定方法.采用18烷基硅烷键合硅胶为填充剂,流动相：乙腈-水（21.5：80.5）,流速1.0ml/min,检测波长283nm.柚皮苷的线性范围为50-800μg/ml,平均回收率98.8%,精密度相对标准偏差（RSD）为0.41%,重现性RSD为1.1%,稳定性RSD值为0.32%.本方法简便、准确,可供本品质量控制. 相似文献
4.
目的：建立乳酸左氧氟沙星氯化钠注射液中主药的含量测定方法。方法：采用反相高效液相色谱法。以Lichrospher5-C18为色谱柱;己烷磺酸钠-甲醇（3：1）为流动相;流速为1．0ml／min;检测波长为293nm,柱温为40℃,进样量为20u1。结果：乳酸左氧氟沙星浓度在5．0-50．0μg／ml内线性关系良好（r=0．9995）,平均回收率为99．85％。RSD为0．25％。结论：此法准确可靠,重现性好,能有效控制乳酸左氧氟沙星氯化钠注射液的质量。 相似文献
5.
建立一种用高效液相色谱法测定茶叶中儿茶素的含量.方法:样品经乙醇提取,超声30min后,过C18小柱净化,样品溶液经0.45μm滤膜过滤后,用于HPLC分析.使用C18(5 um,150 mm×6.0 mm)色谱柱进行分离,用不同体积比混合的流动相A及流动相B的混合液作梯度淋洗,流速为1.0 ml/min,检测波长为280 nm,柱温为40℃.以甲醇∶水∶乙酸-26∶73.5∶0.5(体积比)为流动相.儿茶素在0.02～0.3 g/L范围内线性关系良好,回收率在98.2%～100.3%之间,相对标准偏差为1.6643%.该方法具有操作简便、快速、精密度高、回收率好、重现性较好、检测限低等优点. 相似文献
6.
The cis and trans isomers separation of2-butene- 1,4-diol and lafutidine were studied by HPLC on two kinds of chiral columns: (S,S)-Whelk-O 1 and ChiraSpher. The isomers of 2-butene-1,4-diol can be separated on both chiral columns while the isomers of lafutidine can only be resolved on ChiraSpher column. The influence of different type and amount of mobile phase modifier on the isomers separation was extensively studied. The resolution of cis and trans isomers of 2-butene-1,4-diol was 2.61 on (S,S)-Whelk-O 1 column with hexane-ethanol (97:3, v/v) as the mobile phase. The resolution of lafutidine was 1.89 on ChiraSpher column with hexane-ethanol-THF-diethylamine (92:3:5:0.1, v/v/v/v) as the mobile phase. LC-MS methods were developed to identify the isomer peaks. 相似文献
7.
采用高效液相色谱法对小麦中尿囊素含量进行测定.色谱柱为Kromasil C18,流动相为V甲醇∶V水=5∶95,柱温30℃,流速0.5 mL/min,HPLC测定尿囊素含量变异系数小于1.1%,回收率为95.80%～105.4%,最低检出限0.5μg/mL. 相似文献
8.
Yu Luo Wen-long Li Wen-hua Huang Xue-hua Liu Yan-gang Song Hai-bin Qu 《Journal of Zhejiang University. Science. B》2017,18(5):383-392
A near infrared spectroscopy (NIRS) approach was established for quality control of the alcohol precipitation liquid in the manufacture of Codonopsis Radix. By applying NIRS with multivariate analysis, it was possible to build variation into the calibration sample set, and the Plackett-Burman design, Box-Behnken design, and a concentrating-diluting method were used to obtain the sample set covered with sufficient fluctuation of process parameters and extended concentration information. NIR data were calibrated to predict the four quality indicators using partial least squares regression (PLSR). In the four calibration models, the root mean squares errors of prediction (RMSEPs) were 1.22 μg/ml, 10.5 μg/ml, 1.43 μg/ml, and 0.433% for lobetyolin, total flavonoids, pigments, and total solid contents, respectively. The results indicated that multi-components quantification of the alcohol precipitation liquid of Codonopsis Radix could be achieved with an NIRS-based method, which offers a useful tool for real-time release testing (RTRT) of intermediates in the manufacture of Codonopsis Radix. 相似文献
9.
本文对薄荷—醇—水系统的降温效果在模拟环境条件中作了实验研究。确定出有效的组份配比。并获得明显效果。 相似文献
10.
采用反相高效液相色谱法测定人血清中卡马西平的浓度．人空白血清经处理后,采用高效液相色谱法,C18（4．6mm×250mm,5μm）色谱柱,水-甲醇-乙腈（45：45：10）流动相,UV检测波长254nm,流速1mL·min^-1,柱温：30℃．该方法平均回收率为105．53％,日内和日间RSD均小于11％,标准曲线线性关系良好．该方法适用于临床血药浓度监测． 相似文献
11.
采用依利特色谱柱,乙腈-0.4％磷酸为流动相梯度洗脱,流速1.0 mL/min,检测波长254 nm,柱温40℃,建立热淋清糖浆中没食子酸、原儿茶酸、槲皮苷和槲皮素的高效液相色谱含量测定方法.没食子酸、原儿茶酸、槲皮苷和槲皮素的线性范围分别为1.101～11.008 μg,0.041 6～0.416 0μg,0.045 6～0.455 8 μg,0.006 7～0.067 0μg;平均回收率分别为100.0％（RSD1.3％）、100.0％（RSD1.7％）、100.4％ （RSD1.6％）、100.5％ （RSD2.2％）.所建立的方法准确、稳定,重现性好,可用于热淋清糖浆中有效成分的定量分析. 相似文献
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Chao-hua Tang Jia Liu Qing-yu Zhao Jun-min Zhang 《Journal of Zhejiang University. Science. B》2018,19(6):471-480
A pharmacokinetic comparison of gossypol isomers in cattle was made by investigating their transfer from ingested food to plasma and their degradation by rumen microbes. The gossypol isomers in whole cottonseed, plasma, and rumen fluid were determined by high-performance liquid chromatography (HPLC). The intakes of (+)- and (?)- gossypol by cows on three farms were about 5.6–8.5 and 3.8–5.9 g/(d·herd), respectively. The plasma gossypol concentrations increased as ingestion increased and ranged from 0.31 to 0.48 μg/ml for the (+) form and from 0.39 to 0.59 μg/ml for the (?) form. The (+) form was slightly predominant (58.8%–59.8%) in the gossypol ingested by the cows, whereas the (?) form predominated (54.6%–55.9%) in the plasma. An in vitro study showed that at 6 h, 67.4% and 85.7% of the (?)-gossypol were degraded in 500 and 1000 μg/g treatment groups, respectively, and these increased to 83.6% and 92.5%, respectively, at 12 h. The regularity of the degradation of (+)-gossypol was similar to that of (?)-gossypol. These results showed that (?)-gossypol may be more persistent than (+)-gossypol in plasma, and that the degradation of the gossypol isomers in the rumen is rapid and not enantioselective in cattle. 相似文献
14.
英荣建 《临沂师范学院学报》2008,30(6):72-75
采用超声波法提取了几种松柏科植物中的槲皮素,并用高效液相色谱法（HPLC）分别进行含量的测定．色谱条件如下：C18柱（250×4．6mm,5μm）;流动相为乙腈与0．4％H3PO4的水溶液,比例为40：60;检测波长为360nm;流速为1．0mL·min^-1．实验结果表明,松柏中都含有一定量的槲皮素,柏科植物中槲皮素的含量大约是松科植物的2-5倍,并且其槲皮素的含量随着科属的不同而不同． 相似文献
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阮鸣 《南京晓庄学院学报》2014,(6):50-53
目的：建立高效液相色谱联用示差折光检测器测定冠心宁注射液中果糖、葡萄糖和蔗糖含量的方法.方法：Hanbon Lichrospher NH2分析色谱柱（5μm,4.6×250 mm）,Welchrom氨基保护柱（5μm,10 mm×4.6 mm）,流动相为乙腈—水（70∶30）,柱温：30℃,流速：1.0 ml/min,示差折光检测器设定温度：35℃.结果：回归方程A果糖=85 539C＋677.38,r=0.999 9,A葡萄糖=84 012 C＋575.37,r=1,A蔗糖=187 714C＋504.15,r=1（n=6）,果糖浓度在33.72~1 079μg/ml之间、葡萄糖浓度在32.22~1 031μg/ml之间以及蔗糖浓度在16.19~518μg/ml之间线性关系良好;平均回收率分别为100.1%、100.6%和99.3%,RSD分别为1.99、2.35和2.84%（n=6）;注射液中果糖、葡萄糖和蔗糖的总含量占固含物的55.03%.结论：该方法简便快速、准确可靠,可用于冠心宁注射液中果糖、葡萄糖及蔗糖的含量测定. 相似文献
17.
Shu-fang Wang Jing Leng Yi-min Xu Mei-ling Feng 《Journal of Zhejiang University. Science. B》2013,14(7):604-614
Xiongdankaiming tablet (XDKMT), a well-known compound in traditional Chinese medicine, is widely used for the treatment of acute iridocyclitis and primary open-angle glaucoma. In this paper, accurate and reliable methods were developed for the identification of 20 constituents using high-performance liquid chromatography with photodiode array and electron spray ionization-mass spectrometry (HPLC-PDA/ESI-MS n ), and determination of nine of the constituents (chlorogenic acid, gentiopicroside, isochlorogenic acid B, diosmetin-7-O-β-d-glucopyranoside, apigenin, diosmetin, tauroursodeoxycholic acid, acacetin, and taurochenodeoxycholic acid) was developed using HPLC with ultraviolet absorption detector and evaporative light scattering detector (HPLC-UV/ELSD) for the first time. The best results were obtained on a Zorbax SB-C18 column with gradient elution using water (0.1% formic acid) (A) and methanol (0.1% formic acid) (B) at a flow rate of 0.7 ml/min. Tauroursodeoxycholic acid and taurochenodeoxycholic acid, owing to their low UV absorption, were detected by ELSD. The other seven compounds were analyzed by HPLC-UV with variable wavelengths. The calibration curves of all nine constituents showed good linear regression (R 2>0.9996) within the linearity ranges. The limits of detection and quantification were in the ranges of 0.0460–9.90 μg/ml and 0.115–24.8 μg/ml, respectively. The accuracy, in terms of recovery, varied from 95.3% to 104.9% with relative standard deviations (RSDs) less than 4.4%. Precision (with the intra- and inter-day variations less than 4.4%) was also suitable for its intended use. The developed method was successfully applied for the analysis of major components in XDKMT, which provides an appropriate method for the quality control of XDKMT. 相似文献
18.
采用原位聚合法在石英毛细管内制备了甲基丙烯酸-己二醇二甲基丙烯酸酯（MAA—EDMA）纤维作为同相微萃取（SPME）的萃取头,与高效液相色谱联用测定了环境水样中的多环芳烃．系统考察了萃取时间、解吸时间、盐浓度等实验条件对萃取效率的影响,建立了测定环境水样中的多环芳烃的SPME—HPLC方法．实验结果表明：方法的柱内（n=6）和柱间（n=6）精密度（RSD）分别小于4．45％和5．97％,实际样品的加标回收率在100．8％～108．9％之间;3种多环芳烃化合物的线性范围为10～4000μg／L线性相关系数R2〉0．9496检出限在1．008μg／L～2．876μg／L之间．所制备的Poly（MAA—EDMA）萃取头操作简便、稳定性好、成本低;方法快速、灵敏,适于测定环境水样中的多环芳烃． 相似文献
19.
Kok YY Chu WL Phang SM Mohamed SM Naidu R Lai PJ Ling SN Mak JW Lim PK Balraj P Khoo AS 《Journal of Zhejiang University. Science. B》2011,12(5):335-345
This study aimed to assess the inhibitory activities of methanol extracts from the microalgae Ankistrodesmus convolutus, Synechococcus elongatus, and Spirulina platensis against Epstein-Barr virus (EBV) in three Burkitt's lymphoma (BL) cell lines, namely Akata, B95-8, and P3HR-1. The antiviral activity was assessed by quantifying the cell-free EBV DNA using real-time polymerase chain reaction (PCR) technique. The methanol extracts from Ankistrodesmus convolutus and Synechococcus elongatus displayed low cytotoxicity and potent effect in reducing cell-free EBV DNA (EC(50)<0.01 μg/ml) with a high therapeutic index (>28000). After fractionation by column chromatography, the fraction from Synechococcus elongatus (SEF1) reduced the cell-free EBV DNA most effectively (EC(50)=2.9 μg/ml, therapeutic index>69). Upon further fractionation by high performance liquid chromatography (HPLC), the sub-fraction SEF1'a was most active in reducing the cell-free EBV DNA (EC(50)=1.38 μg/ml, therapeutic index>14.5). This study suggests that microalgae could be a potential source of antiviral compounds that can be used against EBV. 相似文献
20.
建立固相萃取与UPLC—MS／MS检测食品中黄曲霉毒素M1和黄曲霉毒素B1的方法。样品经乙腈提取和SPE小柱萃取净化,提取液经氮气吹干后,用50％甲醇水溶液定容。超高效液相色谱一串联质谱（UPLC—MS／MS）测定,采用电喷雾正离子（ESI＋）模式电离,多反应监测（MRM）模式检测。流动相为0．1％甲酸水溶液和甲醇,流速0．4ml／min,使用ZORBAX Eclipse XDB—C18色谱柱（100mm×3．0mm×1．8μm）为分析柱。黄曲霉毒素AFM1在0．1～50μg／kg范围内线性关系良好、黄曲霉毒素AFB1在0．1～10ug／kg范围内线性关系良好,相关系数均大于0．999;回收率在83．75％～97．8％之间;检出限AFMl为0．05μg／kg、AFBl0．02μg／kg。该法具有分析速度快,检测准确、灵敏度和回收率高等优点,适合食品中黄曲霉毒素M1、B1含量的检测。 相似文献