高效液相色谱-串联质谱法同时测定葛根中葛根素和大豆苷元

提出了高效液相色谱-串联质谱法测定葛根中葛根素和大豆苷元的含量。样品经乙醇提取,所得提取液用乙醇定容至100mL后经Waters Xterra MS C18色谱柱(150mm×3.9mm,5μm)分离,用乙腈与50mmol.L-1甲酸溶液(40+60)的混合液洗脱,采用电喷雾正离子电离多反应监测模式。葛根素和大豆苷元的质量浓度分别在0.050～0.50mg.L-1和5.0～50mg.L-1之间与峰面积呈线性关系,检出限(3S/N)均为5μg.L-1。在0.1,1.0,10.0mg.L-1 3个浓度水平进行加标回收试验,葛根素和大豆苷元的回收率分别为96.6%和97.4%。     

高效液相色谱电化学检测法测定阿奇霉素及相关组分

提出了用高效液相色谱电化学检测法同时测定阿奇霉素颗粒中阿奇霉素(AZMC)及相关组分(即脱糖氧胺阿奇霉素、阿奇霉素A及N-去甲基阿奇霉素)含量的方法.采用Thermo C18柱(150 mm×4.6 mm,5μm)作固定相分离上述4组分.以20 mmol·L-1磷酸二氢钾(用1 mol·L-1氢氧化钾溶液调pH为7.37)-甲醇(47+53)为流动相,流量为1.0 mL·min-1,电化学检测电位为1.05 V,柱温为35℃.阿奇霉素及相关组分的峰面积值与相应浓度之间的线性范围依次为37.06～593.00,2.63～84.00,9.20～294.50,6.69～107.00 mg·L-1,检出限(3S/N)分别为9.28,1.32,4.60,3.35 mg·L-1.用标准加入法作回收试验,测得平均回收率分别为99.9%,100.6%,99.9%,99.8%.     

氨基葡萄糖盐酸盐含量的HPLC柱前衍生法测定

建立了柱前衍生反相高效液相色谱法测定制剂及保健品中的氨基葡萄糖盐酸盐(GAH)的含量,利用邻苯二甲醛与氨基葡萄糖盐酸盐中的氨基进行柱前在线衍生化反应,C18色谱柱洗脱,用荧光检测器(激发340 nm,发射450 nm)测定.流动相A为10 mmol·L-1 Na2HPO4-NaH2PO4缓冲液(pH 7.2,PBS),含0.5%(体积分数)四氢呋喃;流动相B为PBS-甲醇-乙腈(体积比50:35:15).线性范围为1.0 ～100.0 mg·L-1,相关系数为0.999 9,GAH的定量下限为1.0 mg·L-1,保留时间和峰面积的相对标准偏差分别为0.12%和1.69%,加标回收率为99% ～101%.     

高效液相色谱法测定白桦树皮中儿茶素和白桦酯醇的含量

提出了高效液相色谱法(HPLC)测定白桦树皮中白桦酯醇和儿茶素含量的方法.色谱柱为Shim-pack CLC-ODS C18(150 mm×6.0 mm,5 μm),流动相为甲醇-水(75+25)混合溶液,紫外检测波长为205 nm,柱温30℃,流速1.0 mL·min-1,柱压7.747 MPa.儿茶素的线性范围为20.0～400.0 mg·L-1,白桦酯醇的线性范围为15.0～300.0 mg·L-1,儿茶素和白桦酯醇的加标平均回收率分别为95.8%和94.9%,相对标准偏差(n=5)分别为1.67%和2.86%.     

亲水作用色谱法同时测定食品添加剂中D-异抗坏血酸、L-抗坏血酸和二氧化硫脲

食品添加剂样品用含1%(体积分数,下同)甲酸的100mmol·L~(-1)甲酸铵溶液溶解,经乙腈稀释后,用0.22μm微孔滤膜过滤,采用亲水作用色谱法同时测定滤液中D-异抗坏血酸、L-抗坏血酸和二氧化硫脲的含量。以InfinityLab Poroshell 120HILIC-Z色谱柱(3.0mm×100mm,2.7μm)为固定相,以含1%甲酸的100mmol·L~(-1)甲酸铵溶液和乙腈以体积比15∶85组成的混合液为流动相,用二极管阵列检测器测定。D-异抗坏血酸、L-抗坏血酸和二氧化硫脲的质量浓度均在1.0～100mg·L~(-1)内与其对应的峰面积呈线性关系,检出限(3S/N)均为1.0%。以空白样品为基体进行加标回收试验,所得回收率为94.7%～108%,测定值的相对标准偏差(n=6)小于8.0%。     

高效液相色谱法测定保健食品中他达拉非、西地那非、伐地那非违禁药物含量

应用高效液相色谱法测定了保健食品中他达拉非、西地那非、伐地那非等三种违禁药物含量.采用ODS色谱柱,乙腈-0.05 mol·L-1三乙胺(40 60)为流动相,流速1.0 mL·min-1,二极管阵列检测器,检测波长290 am.根据保留时间、光谱图定性,峰高或峰面积定量.该方法三种药物组分在0.5～100.0 mg·L-1浓度范围内呈线性关系,他达拉非和西地那非的检出限为0.3 mg·L-1,伐地那非的检出限为0.4 mg·L-1,相对标准偏差为1.5%～2.0%,回收率为95.8%～107.0%.     

高效液相色谱法同时测定葛枳胶囊中5种有效成分的含量

提出了高效液相色谱法同时测定葛枳胶囊中5种有效成分(葛根素、大豆苷、甘草苷、大豆苷元和甘草酸)的含量。样品经甲醇-水(50+50)溶液超声提取30min,采用Diamonsil C18色谱柱(200mm×4.6mm,5μm)为分离柱,以不同体积比混合的乙腈和磷酸(0.1+99.9)混合液为流动相进行梯度洗脱,甘草苷的检测波长为276nm,其余4种成分均为250nm。5种有效成分分别在一定的质量浓度范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.050～0.338mg·L-1之间。方法的回收率在97.1%～104%之间,测定值的相对标准偏差(n=6)在1.0%～2.7%之间。     

液相色谱-串联质谱法测定葡萄酒中7种生物胺含量

提出了液相色谱-串联质谱法测定葡萄酒中2-苯乙胺、色胺、尸胺、组胺、腐胺、精胺、亚精胺等7种生物胺含量的方法。样品经0.45μm滤膜过滤后,直接通过Zorbax Eclipse XDB C8色谱柱(4.6mm×150mm,5μm)进行分离,以不同体积5mmol·L-1乙酸铵-10mmol·L-1全氟己酸甲醇溶液(A)和5mmol·L-1乙酸铵-10mmol·L-1全氟己酸水溶液(B)的混合液为流动相梯度洗脱,串联质谱法进行测定。7种生物胺的质量浓度均在0.1～5.0mg·L-1范围内与其峰面积呈线性关系,检出限(3S/N)在0.005～0.02mg·L-1之间。以空白葡萄酒样品为基体进行加标回收试验,测得回收率在84.1%～97.5%之间;测定值的相对标准偏差(n=5)在6.3%～13%之间。     

高效液相色谱法测定抗前列腺癌药阿比特龙乙酸酯

提出了高效液相色谱法测定抗前列腺癌药阿比特龙乙酸酯的含量。色谱分离用Amethyst C18-H色谱柱(150mm×4.6mm,5μm),流动相为乙腈-磷酸盐缓冲溶液,流量为1.0mL·min-1,检测波长为236nm,进样量为20μL。阿比特龙乙酸酯的质量浓度在0.1~1.2g·L-1范围内与峰面积呈线性关系,检出限(3S/N)为0.05mg·L-1。以空白样品为基体进行加标回收试验,所得平均加标回收率为99.6%,测定值的相对标准偏差(n=6)为0.17%。     

多菌灵原药中2个酚嗪类杂质含量的高效液相色谱法测定

建立了高效液相色谱法测定多菌灵原药中2个酚嗪类杂质(2,3-二氨基酚嗪(DAP)和2-羟基-3-氨基酚嗪(HAP))含量的方法.采用紫外-可见光检测器,检测波长为453 nm,分析柱为Zorbax SB-C18色谱柱,以甲醇-0.05 mol·L-1乙酸铵溶液(体积比50:50,pH 3.0)为流动相,流速1.0 mL·min-1.DAP在0.136～2.18 mg·L-1质量浓度范围呈线性响应,相关系数为0.999 9,检出限为0.03 mg·L-1,相对标准偏差为1.08%,平均加标回收率为99%;HAP在0.10～1.60 mg·L-1质量浓度范围呈线性响应,相关系数为0.999 9,检出限为0.05 mg·L-1,相对标准偏差为2.71%,平均加标回收率为98%.     

化“材”为“筑”

Chemistry is a central, practical and creative discipline. The development of chemistry plays an important role in the progress of science and society, as well as the improvement of the quality of human life. This paper introduces the chemical knowledge of stone, concrete, glass and other inorganic nonmetallic building materials by the anthropomorphically story. Taking nanomaterials as an example, the prospect of building materials development in the future is put forward.     

"Alpha"-, "beta"- and "delta"-anhydrodigitoxigenin

The syntheses of 3β-hydroxy-5β-carda-14, 20:22-dienolide (= «β»-anhydro-), 3β-hydroxy-5β-carda-8:14, 20:22-dienolide (= «α»-anhydro-) and «δ»-anhydro-digitoxigenin (= probably 3β-hydroxy-5β, 14β-carda-8, 20:22-dienolide) by the best ways known to date, have been described. «δ»-Anhydro-digitoxigenin represents the thermodynamically most stable isomer. In this isomer the double bond in position 8 is unaffected by hydrogenation with Pt in acetic acid; with perbenzoic acid an epoxide results from which, on hydrogenation, the double bond can be regenerated in its original position. Analogous reactions are known to occur in the 8:14-epoxides.     

Making "wheels" and "cubes" from triangles

[Mn(IV)Mn(II)3] triangular units directed by the presence of tripodal alcohols self-assemble in the presence of azide and acetate ligands to form either a [Mn24] "wheel" or a [Mn32] "cube".     

"Turn-on" fluorescent sensing with "reactive" probes

Chemical probes are valuable tools for the investigation of biochemical processes, diagnosis of disease markers, detection of hazardous compounds, and other purposes. Therefore, the development of chemical probes continues to grow through various approaches with different disciplines and design strategies. Fluorescent probes have received much attention because they are sensitive and easy-to-operate, in general. To realize desired selectivity toward a given analyte, the recognition site of a fluorescent probe is designed in such a way to maximize the binding interactions, usually through weak molecular forces such as hydrogen bonding, toward the analyte over other competing ones. In addition to such a supramolecular approach, the development of fluorescent probes that sense analytes through chemical reactions has witnessed its usefulness for achieving high selectivity, in many cases, superior to that obtainable by the supramolecular approach. Creative incorporations of the reactive groups to latent fluorophores have provided novel chemical probes for various analytes. In this feature article, we overview the recent progress in the development of turn-on fluorescent probes that are operating through chemical reactions triggered by target analytes. Various chemical reactions have been implemented in the development of many reactive probes with very high selectivity and sensitivity toward target analytes. A major emphasis has been focused on the type of chemical reactions utilized, with the hope that further explorations can be made with new chemical reactions to develop reactive probes useful for various applications.     

"Clickable" polymersomes

Polymersomes, composed of amphiphilic polystyrene-block-poly(acrylic acid) (PS-b-PAA), with the periphery being covered with azide groups, were used for further functionalization using "click" chemistry.