Analysis of steroidal glycoalkaloids and their metabolites in Solanum nigrum fruits based on liquid chromatography-tandem mass spectrometry and molecular networking

Solanum nigrum fruit is like a treasure house for anticancer drugs because of its steroidal alkaloids. However, the clinical treatment of cancer mainly uses immature fruits, which can cause a toxic reaction if eaten directly, while mature fruits are eaten as fruit. In order to clarify the reasons for the differences in pharmacodynamics and toxicity between them, we studied the composition and metabolism of steroidal alkaloids in fruits of different maturities based on liquid chromatography-tandem mass spectrometry and molecular networking. As a result, 114 steroidal glycoalkaloids were identified. During fruit ripening, the aglycones of steroidal alkaloids mainly undergo hydroxylation and carboxylation, and the sugar side chains mainly undergo acylation and glycosylation reactions. Furthermore, 219 steroidal alkaloids were identified in a metabolism experiment in rats. Metabolic processes include deglycosylation, redox, sulfuric acid binding, acetyl binding, and glucuronic acid-binding. Steroidal alkaloids in mature fruits have high molecular weight and polarity, which are difficult to absorb, and most of them are excreted through feces and urine, which may be the reason for their poor efficacy. This study lays a foundation for research on the biosynthesis of steroidal alkaloids and provides potential candidates for the discovery of new steroidal alkaloid anticancer drugs.     

Analysis of pesticide residues in fruit and vegetables with ethyl acetate extraction using gas and liquid chromatography with tandem mass spectrometric detection

A multiresidue method based on extraction with ethyl acetate has been used at the Swedish National Food Administration since 1989 to monitor pesticide residues in fruit and vegetables. The method has been continuously adjusted, resulting in simple and quick analyses of pesticide residues. To recover basic pesticides, the addition of an alkali is necessary. The addition of sodium hydrogen carbonate has been shown to recover all pesticides effectively without any degradation. The liquid chromatography (LC) with tandem mass spectrometry (MS/MS) technique has made it possible to analyse more polar pesticides and to replace many single methods. The latest development in the multiresidue method, comprising the use of gas chromatography (GC) with MS/MS, has further improved the analysis by replacing the conventional GC detectors. The need for cleanup has been reduced or eliminated entirely. Consequently, the method has been simplified in a way that makes it possible to recover all included analytes in many different matrices in one single extraction and to detect them either with GC-MS/MS or with LC-MS/MS.     

Chemical screening of olive biophenol extracts by hyphenated liquid chromatography

Chemical screening using reversed phase HPLC-photodiode array detection (RPLC-DAD) and RPLC-electrospray ionisation mass spectrometry (RPLC-ESI-MS) is widely applied as an approach to streamline natural products research. The full potential of this approach is demonstrated in this paper by application to the chemical screening of olive products including olive mill waste (OMW). Out of 100 biophenols previously reported in olive products, the on-line RPLC-DAD-ESI-MS was able to confirm the presence of 52 compounds in OMW. This included a number of simple phenols, flavonoids and secoiridoids. By careful examination of the combined DAD and ESI-MS data, extra information was elucidated including: the site of glycosidation on the phenol ring of hydroxytyrosol; the identity of the other luteolin-glucoside isomer as luteolin-4′-O-glucoside; identifying rutin rather than the previously reported hesperidin (and the reasons for possible mis-assignment); and the detection of diastereomers of 4-hydroxyphenylethyl alcohol-deacetoxy elenolic acid dialdehyde (4-HPEA-DEDA) and 3,4-dihydroxyphenylethyl alcohol-deacetoxy elenolic acid dialdehyde (3,4-DHPEA-DEDA).     

微波场协同提取红龙果食用红色素的研究

研究了应用微波从红龙果（Hylocereus Costaricensis or Weber Britt）中提取食用红色素的新工艺，并确定了最佳工艺条件：提取剂为50％的乙醇溶液，原料用量（g）与提取剂用量（mL）比为1：90。微波功率为700W，提取时间为20s，提取次数为4次。最佳工艺条件下的色素提取率为98．94％，产品pH值为6。与溶剂浸提法相比，微波法提取红龙果食用红色素的每次提取时间由2h减少到20s，提取率从90．96％增加到98．94％。     

Determination of the carbon-13 content of sugars and pulp from fruit juices by isotope-ratio mass spectrometry (internal reference method). A European interlaboratory comparison

An interlaboratory comparison by ¹³C-isotope ratio mass spectrometry was organised by working group No. 1 of the European Commission of Standardisation (CEN/TC 174) in order to define the repeatability (r) and the reproducibility (R) of the ¹³C determination in sugars and pulp, isolated from the same fruit juice. Six unlabelled juices were analysed in 19 laboratories in the European Union, Australia and the USA. Three samples were authentic juices (orange, grapefruit, pineapple) and the remaining samples were the same juices with an addition of sugar at 15 g l⁻¹ (orange, pineapple) or 11.8 g l⁻¹ (grapefruit). The sugar was prepared by mixing equal amounts of beet and cane sucroses. The different laboratories used the same experimental protocol under different conditions (operator, conversion system for CO₂ preparation, mass spectrometer). The results for the sugars (r = 0.27%., R = 0.82%.) were comparable to those from an earlier ring test (r = 0.30%., R = 0.70%.), while the results for the pulp presented higher interlaboratory variability (r = 0.38%., R = 1.89%.) possibly due to experimental difficulties. Nevertheless, the RSD_R for free sugars ranged 0.9–3.2% and for pulp, 0.9–9.3%. On the basis of the Horwitz equation and taking account of the concentration of the isotopes measured, an RSD_R of 7–8% might have been expected. The experimentally determined RSD_R values were less than twice the theoretically expected values, which is a criterion of an acceptable method. The results were therefore considered to be acceptable by specialists in the field of isotopic analysis, and the method applied was found to improve the sensitivity of the ¹³C determination for the detection of sugar addition in fruit juices.     

气相色谱/质谱法分析曼陀罗果实挥发油的化学成分

用水蒸汽蒸馏法从曼陀罗果实中提取挥发油,并用气相色谱/质谱(GC/MS)联用技术对其化学成分进行分离和结构鉴定,用峰面积归一化法确定各成分的相对含量。结果确定了68种化合物,占挥发油总量的82.83%,其主要成分为6-戊基-5,6-二氢化吡喃-2-酮(9.13%)、3,7,11,15-四甲基-2-十六碳烯-1-醇(6.71%)、二苯酮(6.16%)和1-己醇(6.10%)等。     

果皮厚度对水果组织中光传输特性的影响

水果产品品质检测技术在水果的生产和消费中起着十分重要的作用。利用水果产品的光学特性进行无损检测是水果品质无损检测与分级技术中最实用的和最成功的技术之一。深入研究光在水果组织中的输运规律,对于水果产品品质的光学检测有着十分重要的意义。本文以仁果类薄皮水果苹果和厚皮水果柑橘为例,建立果皮和果肉两层组织模型,利用蒙特卡罗法模拟了808 nm的波长下高斯光束在水果组织中传输的光学特性,揭示了水果果皮厚度对光在组织中的传输特性如漫反射率、透射率、内部吸收率和穿透深度等特性的影响,分析了果肉组织的检测效率。研究结果表明,果皮越厚,透射率和穿透深度越小,果皮比果肉的光吸收能量密度在径向距离上的分布范围更广,随着水果组织内部深度的增加,光吸收能量密度逐渐减小,径向方向减弱的更快。而对于漫反射率,在径向距离0.2～1.2 cm之间,果皮越薄漫反射率越小,在1.2～4.0 cm之间,果皮越厚漫反射率越小。此研究结果表明在用光学检测方法对水果进行无损检测和分级时,无论是透射或反射测量,果皮厚度和光束的相互作用都不应忽视,也为不同类型的水果产品设计更为有效的光学检测装置(如光源的强度、检测器的大小以及位置等)提供了理论基础,对于水果产品品质的光学检测有着十分重要的意义。     

烟用香料无花果提取物的热裂解产物研究

为了评价无花果提取物在卷烟加料中的使用效果,采用热裂解-气相色谱-质谱联用(PY-GC-MS)方法对无花果提取物的热裂解产物进行剖析.结果表明无花果提取物热裂解后产生大量醛类、酮类和呋喃类物质,这些物质是构成卷烟香味的重要成分,能有效改善卷烟吸味.     

不同红梨品种果实中营养元素含量的光谱测定

用火焰原子吸收光谱法对美人酥、红酥脆和满天红3个红梨品种果实中K,Fe,Zn,Ca,Cu,Mg和Mn七种营养元素含量进行了测定分析。各元素在实验范围内,线性关系良好,回收率在98%～104%之间,结果较为满意。3个红梨品种果实中均含有丰富的营养元素,且含量均是K＞Fe＞Zn＞Ca＞Cu＞Mg＞Mn。不同品种果实中,K,Zn,Mg和Mn含量为美人酥＞红酥脆＞满天红;Fe和Cu含量为红酥脆＞满天红＞美人酥;Ca含量为满天红＞红酥脆＞美人酥;七种营养元素总量为红酥脆＞美人酥＞满天红。     

高效液相色谱法测定果酸

本文研究了反相高效液相色谱法同时分离和测定6种果酸的色谱条件,提出了有效提取果酸的方法,并对苹果梨、香水梨等样品进行了实际分析。结果表明,该法简更快速,具有较高的准确度和精密度。