Quantitative Determination of Busulfan in Human Plasma by UPLC

A rapid and reliable UPLC method was developed and validated for the determination of busulfan in human plasma. After protein precipitation, derivatization, and liquid–liquid extraction, separation of derivatized busulfan was achieved on an Acquity BEH C₁₈ column using a gradient mobile phase consisting of a trifluoroacetic acid aqueous solution (0.2%, v/v) and acetonitrile. The column temperature was maintained at 50 °C and UV detection was carried out at 254 nm. The complete analytical run time was 1.3 min, 7-fold faster than our previous LC methodology. Quantification was performed using external standardization and calibration curves were linear (r ≥ 0.999) over the dynamic range of 0.05–5.00 μg mL⁻¹. Intra-day and inter-day coefficients of variation were ≤6.9 and 3.9%, respectively, across the range of concentrations. Accuracy of the analytical method expressed as the relative error percentage was better than 5.4%. LOD and LOQ were 0.013 and 0.025 μg mL⁻¹, respectively. Data obtained using the UPLC method was compared to those obtained from our previously used LC method by Deming regression analysis. The UPLC method was accurate, sensitive, and greatly increased sample analysis throughput as compared to our previous LC methodology allowing for a 4-fold increase in the number of patients who could be monitored during transplant therapy.

     

Determination of Ruscogenin in Turkish Ruscus L. Species by UPLC

Determination of ruscogenin in five Ruscus taxa in Turkey was performed by ultra performance liquid chromatography (UPLC). Chromatographic separation and determination of ruscogenin in herb and rhizome samples were accomplished on an Acquity UPLC^TM BEH C₁₈ (50 mm × 2.1 mm, i.d., 1.7 μm) column system using an isocratic elution with a mobile phase consisting of acetonitrile and water (90:10) (v/v) at a constant flow rate of 0.3 mL min⁻¹. Chromatographic calibration graph of ruscogenin in the concentration range of 22–55 μg mL⁻¹ was obtained by using the linear relationship between the concentration and the peak area measured at a wavelength of 200 nm. The method was validated and successfully applied to the quantitative analysis of the real samples containing ruscogenin of Ruscus species. The ruscogenin amount in the hydrolyzed herb of Ruscus aculeatus was higher than in the hydrolyzed rhizomes of Ruscus aculeatus. In the rhizomes of R. colchicus, R. hypoglossum and R. hypophyllum, the ruscogenin amount was higher than in the herbs.

     

反相高效液相色谱法测定大蒜中蒜氨酸的含量

大蒜为百合科葱属植物蒜AlliumSativumLinn .的鳞茎。有关大蒜中蒜氨酸的含量,文献[1,2 ]中均由大蒜辣素的含量来推测。最新的美国药典[3 ] 采用衍生化法测定大蒜中的蒜氨酸,操作麻烦,气味难闻。本文报道的不需衍生化的高效液相色谱法,操作简单,线性关系良好,结果准确。1　实验     

Mit der Analyse der ?therischen ?le von Allium sativum L.

Ohne Zusammenfassung     

Comparative studies of bioactive organosulphur compounds and antioxidant activities in garlic (Allium sativum L.), elephant garlic (Allium ampeloprasum L.) and onion (Allium cepa L.)

We evaluated organosulphur compounds in Allium vegetables, including garlic, elephant garlic and onion, using high-performance liquid chromatography. Among organosulphur compounds, elephant garlic had considerable γ-glutamyl peptides, and garlic had the highest alliin content. Onion had low level of organosulphur compounds than did elephant garlic and garlic. In addition, antioxidant capacities were evaluated by oxygen radical absorbance capacity (ORAC) values and 2,2-diphenyl-1-picrylhydrazyl (DPPH) and 2,2′-azinobis(3-ethylbenzothiazoline-6-sulphonic acid) (ABTS) radical scavenging assay. The results showed that garlic had the highest antioxidant capacity, followed by elephant garlic and onion. Furthermore, a positive correlation was observed between antioxidant activities and organosulphur compounds (R > 0.77). Therefore, our results indicate that there was a close relationship between antioxidant capacity and organosulphur compounds in Allium vegetables.     

Determination of Organophosphorus Pesticides in Leeks (Allium porrum L.) by GC-FPD

A method was validated for the analysis of organophosphorus pesticides in leeks. The leek sample was cut into about 2 cm lengths and heated in a microwave oven for 50 s to inactivate enzymes. The sample was extracted with 50 mL acetonitrile using an Ultra-turrax T18 blender and cleaned up by solid phase extraction. The target analytes were determined by GC with a flame photometric detector. Average recoveries were 73–118% and limits of detection ranged from 1.1 to 10.0 μg kg^?1. The uncertainty of the analysis for each pesticide was evaluated as below 16%. The method was applied to determine organophosphorus pesticides in real samples. The GC–MS was used as confirmatory tool for positive samples.     

大蒜素的检测及大蒜辣素分解机理的探讨

通过正交试验方法,研究了硫酸钡吸光比浊法测定大蒜中大蒜素含量的最佳实验条件。在选定实验条件下,体系的吸光度与硫酸根离子浓度呈线性关系,相关系数r为0.9985,相对标准偏差(RSD)为0.86%。采用高效液相色谱法对样品中二烯丙基二硫醚进行定量检测,其检测结果与吸光比浊法的结果具有一定的互补对照性。在此基础上采用红外光谱法、气相色谱-质谱法对大蒜素中含硫活性成分进行定性分析,并将四种方法结果进行对比,对大蒜辣素过热分解的机理进行了探讨,为大蒜素中不同含硫化合物之间的转化提供了依据。     

薄层扫描法测定挥发大蒜油中的大蒜辣素

挥发大蒜油在薄层板上分离出的最大斑点的化学成分用红外光谱法定性,用薄层扫描法定量。大蒜辣素在0．667-1．112μg范围内峰面积和质量的线性关系良好(r=0．9988),方法的平均回收率为98．4％,RSD=0．59％(n=5)。实验结果表明这种方法简便、快捷、准确。     

火焰原子吸收光谱法测定不同产地大蒜中11种金属元素的含量

为进一步利用和开发大蒜资源,采用V（硝酸）＋V（高氯酸）=4＋1常压微沸条件下消化,用火焰原子吸收法测定不同产地大蒜中的金属元素Na、Ca、Mg、Mn、Cu、K、Zn、Fe、Cr、Cd和Pb的含量。研究了不同元素的仪器最佳工作条件,并做了准确度和精密度的考察。结果表明,大蒜中Na、Ca、Mg、Mn、Cu、K、Zn、Fe、Cr、Cd和Ph的含量分别为236．49、1598．21、612.44, 6.27, 15.48, 12 172.41, 126.88, 64.46, 1.67, 1.75, 2.02; 172.84, 1 243.38, 610.05, 5.32, 13.60, 11689.65, 120. 07, 78.91, 1.75, 2. 04, 1.97; 136. 90, 1467.93, 574. 16, 6. 27,16.90, 12 263.45, 146.34, 116.20, 1.82, 2.17, 2.25 μg·g^-1。加标回收率为96．60％～105．80％,相对标准偏差（n=9）为：0．24％～4．81％,测定方法简单易行,方便快捷。     

超高效液相色谱法测定橡胶中6种橡胶助剂的含量

取条状橡胶样品(厚约2mm,宽约1mm)1.000g,加入体积比为6∶1的乙腈-二氯甲烷混合溶液50mL,超声提取60min,所得溶液经0.45μm滤膜过滤,滤液用于超高效液相色谱法分析。用ZORBAX Eclipse XDB-C18色谱柱(4.6mm×100mm,1.8μm)为固定相,以体积比为40∶60的乙腈-pH 4.0的12.5mmol·L^-1磷酸二氢钠混合溶液为流动相进行等度洗脱,使所测定的6种橡胶助剂得以分离,对6种橡胶助剂在不同波长处进行紫外检测,防老剂6PPD[N-(1,3-二甲基)丁基-N′-苯基对苯二胺]的检测波长为290nm,防焦剂CTP(N-环己基硫代邻苯二甲酰亚胺)和其他4种硫化促进剂[TBBS(N-叔丁基-2-苯并噻唑次磺酰胺)、MBTS(2,2-二硫化二苯并噻唑)、CBS(N-环己基-2-苯并噻唑次磺酰胺)、DCBS(N,N-二环己基-2-苯并噻唑次磺酰胺)]的检测波长均为226nm。6种橡胶助剂的标准曲线的线性范围均为5.0~500.0mg·L^-1,其检出限(3S/N)为0.3~2.5mg·L^-1。按标准加入法进行回收试验,测得回收率为82.8%~107%,测定值的相对标准偏差(n=5)均小于5.0%。     

GC-MS法测定大蒜中的挥发性物质

大蒜(AlliumsatiuvmL.)是多年生草本百合科植物大蒜的鳞茎,按皮的颜色不同可分为紫皮蒜和白皮蒜两种。大蒜原产于意大利的西西里岛,约在两千多年前传入我国。大蒜不仅是极佳的调味食品,而且还有很好的药用功能。近年来,科学家研究证明,大蒜是一种健康食品,有助人体防病保健、延年益寿,是药食兼优的佳品,对人体具有多种药用价值。大蒜具有一种强烈的蒜臭气味,这种特殊的气味由许多复杂的硫化物组成。这类有机硫化物可促进消化,健胃整肠,强化抗菌作用,消肿止痛,改善机体机能的功能,大蒜中还含有乙烷硫代磺酸乙酯和二烯丙基三硫化物等,能阻断强烈致癌物质亚硝胺类在胃部的形成和积累,可预防胃癌、食道癌、肝癌、鼻咽癌的发生。本试验采用"同时蒸馏-萃取方法"(simultaneousdistillationandextraction,SDE)提取白皮和紫皮大蒜的挥发性成分,经GC-MS分析,确定了化合物的化学组成和相对百分含量。     

Comprehensive Metabolite Profiling in Genetic Resources of Garlic (Allium sativum L.) Collected from Different Geographical Regions

Garlic (Allium sativum) is the second most important Allium crop that has been used as a vegetable and condiment from ancient times due to its characteristic flavor and taste. Although garlic is a sterile plant that reproduces vegetatively through cloves, garlic shows high biodiversity, as well as phenotypic plasticity and environmental adaptation capacity. To determine the possible mechanism underlying this phenomenon and to provide new genetic materials for the development of a novel garlic cultivar with useful agronomic traits, the metabolic profiles in the leaf tissue of 30 garlic accessions collected from different geographical regions, with a special focus on the Asian region, were investigated using LC/MS. In addition, the total saponin and fructan contents in the roots and cloves of the investigated garlic accessions were also evaluated. Total saponin and fructan contents did not separate the garlic accessions based on their geographical origin, implying that saponin and fructan contents were clone-specific and agroclimatic changes have affected the quantitative and qualitative levels of saponins in garlic over a long history of cultivation. Principal component analysis (PCA) and dendrogram clustering of the LC/MS-based metabolite profiling showed two major clusters. Specifically, many Japanese and Central Asia accessions were grouped in cluster I and showed high accumulations of flavonol glucosides, alliin, and methiin. On the other hand, garlic accessions grouped in cluster II exhibited a high accumulation of anthocyanin glucosides and amino acids. Although most of the accessions were not separated based on country of origin, the Central Asia accessions were clustered in one group, implying that these accessions exhibited distinct metabolic profiles. The present study provides useful information that can be used for germplasm selection and the development of new garlic varieties with beneficial biotic and abiotic stress-adaptive traits.     

Determination of the volatile constituents of ChineseCoriandrum sativum L. by gas chromatography—Mass spectrometry with solid-phase microextraction

Summary Fifteen main volatile compounds in ChineseCoriandrum sativum L. were separated and identified by gas chromatography—mass spectrometry (GC-MS) combined with solid-phase microextraction (SPME). Fresh ChineseCoriandrum sativum L. was ground and its volatile compounds were extracted by SPME with a 100 μm polydimethylsiloxane fiber. The fibers were desorbed in a GC injection liner at 250°C for 3 min. More than 15 peaks were separated by headspace SPME-GC-MS analysis. The main compounds in headspace ofCoriandrum sativum L. identified by mass spectrometry included decanal, 2-decenal, 1-decanol,trans-2-decen-1-ol,trans-2-decen-1-al,trans-2-tridecenal etc, which were verified by reference compounds. Their relative contents were calculated on basis of peak areas. SPME extraction conditions and capillary chromatography column used to separate the volatile compounds were investigated.     

UPLC法测定浓缩苹果汁中阿维菌素残留量

建立了超高效液相色谱法(UPLC)测定浓缩苹果汁阿维菌素残留的方法。样品经C18固相萃取柱(250×4.6μmi.d.,5 mm)净化分离,以V(乙腈)∶V(水)=80∶20为流动相,245 nm波长检测,流速0.3 mL/min。结果表明:本法测定的阿维菌素在4 min内可以完全分离,线性范围为0.01~200 mg/L,R2=0.9997,当添加量为0.05、0.5、1.0 mg/kg时,回收率为99.5%~108.1%,RSD为0.30%~1.1%,测定下限为0.005 mg/kg。方法可用于浓缩苹果阿维菌素残留量测定。     

Solvent Mixture Optimization in the Extraction of Bioactive Compounds and Antioxidant Activities from Garlic (Allium sativum L.)

Garlic is a health promoter that has important bioactive compounds. The bioactive extraction is an important step in the analysis of constituents present in plant preparations. The purpose of this study is to optimize the extraction with the best proportion of solvents to obtain total phenolic compounds (TPC) and thiosulfinates (TS) from dried garlic powder, and evaluate the antioxidant activities of the optimized extracts. A statistical mixture simplex axial design was used to evaluate the effect of solvents (water, ethanol, and acetone), as well as mixtures of these solvents, after two ultrasound extraction cycles of 15 min. Results showed that solvent mixtures with a high portion of water and pure water were efficient for TPC and TS recovery through this extraction procedure. According to the regression model computed, the most significant solvent mixtures to obtain high TPC and TS recovery from dried garlic powder are, respectively, the binary mixture with 75% water and 25% acetone and pure water. These optimized extracts presented oxygen radical absorbance capacity. Pure water was better for total antioxidant capacity, and the binary mixture of water–acetone (75:25) was better for DPPH scavenging activity. These optimized extracts can be used for industrial and research applications.     

超高效液相色谱法测定进出口浓缩苹果汁中的吡虫啉残留量

建立了超高效液相色谱法(UPLC)测定浓缩苹果汁中吡虫啉残留量的方法.优化了样品前处理方法及UPLC分离测定条件.样品与饱和NaCl水溶液混合后,经石油醚除杂,V(乙腈):V(CH2Cl2)=90:10萃取.结果表明:在优化条件下,本法测定吡虫啉的线性范围为0.025～5.0 μg/mL,检出限0.005 mg/kg,平均加标回收率为91.3%,其线性方程为Y=9015.2ρ+131.59,R2=0.9990.该方法可满足进出口浓缩苹果汁中吡虫啉检测的要求.     

Simultaneous Determination of Ten Antibiotic Residues in Milk by UPLC

An analytical method for rapid screening and quantitative determination of ten antibiotics (chloramphenicol, thiamphenicol, tetracycline, oxytetracycline, chlortetracycline, metacycline, doxycycline, cefoperazone, ceftriaxone and cefaclor) residues in milk was developed using ultra performance liquid chromatography with photodiode array detector. After extraction with McIIvaine buffer + methanol (8 + 2), the extract was cleaned up with solid-phase extraction cartridge. The conditions of sample extraction, cleaning and separation were optimized. The average spiked recoveries of milk samples were 52.1–68.0, 70.1–81.0 and 76.2–101.0% at spiked levels of 0.1, 0.5, 2.5 μg g^?1, respectively with precisions of 3.3–15.9%. The limits of detection and quantification were 0.003–0.022 and 0.01–0.08 μg g^?1, respectively. The proposed method has been applied to the determination of antibiotics in actual milk samples with satisfactory results.     

电感耦合等离子体原子发射光谱法测定新疆洋葱籽中常量/微量元素

采用微波消解法处理样品,以电感耦合等离子体原子发射光谱法(ICP-AES)测定新疆洋葱籽样品中Co、Cr、Ca、K、Mg、P、Fe、Mn、Na、Ni、Sn、Zn、Cd、As、Se、Cu、Mo和V 18种常量/微量元素。结果显示,新疆洋葱籽中含有丰富的K、Mg、P、Ca和Na等常量元素,此外微量元素Fe、Mn、Zn、Cr、Ni、Cu的含量也较丰富。新疆洋葱籽中含有很多对人体有益的常量及微量元素,有较高的药用价值。