Yellow sarson(Brassica rapa ssp. trillocularis) is an important rapeseed-mustard species of Brassica rapa due to its high seed oil content. Glycerolipids and fatty acid composition affect seed germination and determin...Yellow sarson(Brassica rapa ssp. trillocularis) is an important rapeseed-mustard species of Brassica rapa due to its high seed oil content. Glycerolipids and fatty acid composition affect seed germination and determine the quality of seed oil. To date, no information is available on the composition of individual glycerolipids in this species. Therefore, in this study the glycerolipid profiling of yellow sarson seeds was performed using ultra high performance liquid chromatography coupled to triple time-of-flight mass spectrometry(UPLC-Triple-TOF-MS).A fast and efficient chromatographic separation of glycerolipids was accomplished based on an UPLCTMBEH C8 column within 22 min.In ESI positive ion mode, TOF-MS scan-information dependent acquisition-product ion scan was carried out to acquire both high resolution MS and MS/MS information from one injection. According to MS/MS spectra, predominant fragmentation patterns of glycerolipids were elucidated in detail. Based on retention time, accurate mass, isotopic distribution, and fragmentation patterns, the composition of 144 glycerolipids and fatty acids were finally identified in yellow sarson seeds, including 77 triacylglycerols, 32 diacylglycerols, 18sulfoquinovosyl-diacylglycerols, 5 monogalactosyl-diaclyglycerols, and 12 digalactosyl-diacylglycerols. Of them, the most abundant glycerolipids in yellow sarson seeds were triacylglycerols, the major storage form of seed oil in plants. In addition, diacylglycerols were found as a minor component of glycerolipids. The lowest amounts of glycerolipids detected in seeds were glycosyl-acylglycerols. The results revealed the composition and relative content of glycerolipids in yellow sarson seeds, which will provide a more comprehensive assessment of the quality of seed oil and also help to select functional cultivars with higher beneficial glycerolipids. This profiling method has the advantages of high throughput, high sensitivity and good accuracy, which will provide a reliable analysis platform for glycerolipids metaboli展开更多
文摘目的:利用诊断离子建立了一个磷酸二酯酶-5(PDE5)型抑制剂的非目标扫描策略,通过高效液相色谱-四极杆飞行时间质谱(HPLC-QTOF/MS)1次扫描即能完成中药及保健食品中添加的PDE5型抑制剂的筛查。方法:采用Poroshell EC-C18色谱柱,以0.1%乙酸-乙腈为流动相,梯度洗脱,流速为0.3 m L·min-1;采用电喷雾离子源(ESI),毛细管电压3.5 k V,碎裂电压180 V,在自动扫描模式下,对不同类型PDE5型抑制剂的裂解规律进行分析,从中寻找诊断离子建立非目标扫描策略。对MS条件进行优化,讨论了筛查策略参数对结果的影响。结果:11种典型PDE5抑制剂质量浓度在50~1 000 ng·m L-1范围内线性关系良好;平均回收率为83.7%~110.0%,RSD为1.5%~10.2%。对25批样品进行筛查,结果与目标扫描策略一致,但是诊断离子策略能够更有效地发现未知衍生物。结论:该方法简可用于已知及未知的非法添加PDE5型抑制剂的快速筛查。
基金supported by the National Risk Assessment Project for the Project of Risk Assessment on Vegetable Products (GJFP2017002)the Basic Scientific Research Project of Institute of Vegetables and Flowers, Chinese Academy of Agricultural Sciences (1610102016023)
文摘Yellow sarson(Brassica rapa ssp. trillocularis) is an important rapeseed-mustard species of Brassica rapa due to its high seed oil content. Glycerolipids and fatty acid composition affect seed germination and determine the quality of seed oil. To date, no information is available on the composition of individual glycerolipids in this species. Therefore, in this study the glycerolipid profiling of yellow sarson seeds was performed using ultra high performance liquid chromatography coupled to triple time-of-flight mass spectrometry(UPLC-Triple-TOF-MS).A fast and efficient chromatographic separation of glycerolipids was accomplished based on an UPLCTMBEH C8 column within 22 min.In ESI positive ion mode, TOF-MS scan-information dependent acquisition-product ion scan was carried out to acquire both high resolution MS and MS/MS information from one injection. According to MS/MS spectra, predominant fragmentation patterns of glycerolipids were elucidated in detail. Based on retention time, accurate mass, isotopic distribution, and fragmentation patterns, the composition of 144 glycerolipids and fatty acids were finally identified in yellow sarson seeds, including 77 triacylglycerols, 32 diacylglycerols, 18sulfoquinovosyl-diacylglycerols, 5 monogalactosyl-diaclyglycerols, and 12 digalactosyl-diacylglycerols. Of them, the most abundant glycerolipids in yellow sarson seeds were triacylglycerols, the major storage form of seed oil in plants. In addition, diacylglycerols were found as a minor component of glycerolipids. The lowest amounts of glycerolipids detected in seeds were glycosyl-acylglycerols. The results revealed the composition and relative content of glycerolipids in yellow sarson seeds, which will provide a more comprehensive assessment of the quality of seed oil and also help to select functional cultivars with higher beneficial glycerolipids. This profiling method has the advantages of high throughput, high sensitivity and good accuracy, which will provide a reliable analysis platform for glycerolipids metaboli