GC/GCMS analysis of the petroleum ether and dichloromethane extracts of Moringa oleifera roots

Objective:To explore the phytochemical constituents from petroleum ether and diehloromethane extracts of Moringa oleifera(M.oleufera)roots using GC/GC—MS.Methods:A total of 5.11 kg fresh and undried crashed root of M.oleifera were cut into small pieces and extracted with petroleum ether and diehloromethane(20 L.each) at room temperature for 2 d.The concentrated extracts were subjected to their GC—MS analysis.Results:The GC-MS analysis of the petroleum ether and diehloromethane extracts of M.oleifern roots,which showed promising biological activities,has resulted in the identification 102 compounds.These constituents belong to 15 classes of compounds including hydrocarbons,fatty acids,esters,alcohols,isolhioeyanate.thiocyanale,pyrazine,aromalics.alkamides.cyanides,steroids,halocompounds.urea and N-hydroxyimine derivatives,unsaturated alkenamides.alkyne and indole.GC/GC-MS studies on petroleum ether extraet of the roots revealed that it contained 39 compounds,belonging to nine classes.Cyclooctasulfur S8 has been isolated as a pure compound from the extract.The major compounds identified from petroleum ether extract were trans-13-clocosene(37.9%).nonacosane(32.6%).cycloartenol(28.6%) nonadecanoic acid(13.9%) and cyclooctasulfur S8(13.9%).Dichloromethane extract of the roots was composed of 63 compounds of which nasimizinol(58.8%) along with oleic acid(46.5%),N—benzyl-N-(7—cyanato heptanamide(38.3%),N—benzyl-N—(1—chlorononyl) amide(30.3%),bis[3—benzyl prop-2-ene]-1-one(19.5%) and N.N-dibeuzyl—2-ene pent 1.5—diamide(11.6%) were the main constituents.Conclusions:This study helps to predict the formula and structure of active molecules which can be used as drugs.This result also enhances the traditional usage of M.oleifera which possesses a number of bioactive compounds.

Spectral Properties of Extracted Complexes of MetalPicrates with Crown Ethers

The investigation on UV-visible spectra of species formed by extracting some metal picrates with benzo-15-crown-5(B15C5) and dibenzo-18-crown-6(DB18C6) verified that there are some interactions of picrate anion with K+, Na+ and rare earth ions in loaded organic phase. By the study of the charge transfer band and absorption spectra of picrate anion, it can be determined whether an ion pair has been formed and either a 1 : 1 contact ion pair or a 1 : 2 crown-separated ion pair involved in organic phase can be distinguished for an ion-pair extraction.

An Electrochemical Understanding of Extraction of Silver Picrate by Benzo-3<i>m</i>-Crown-<i>m</i>Ethers (<i>m</i>= 5, 6) into 1,2-Dichloroethane and Dichloromethane

Two extraction constants (Kex± and Kex) for extraction of silver picrate (Ag﹢Pic﹣) by benzo-15-crown-5 ether (B15C5) and benzo-18-crown-6 one (B18C6) into 1,2-dichloroethane (DCE) and dichloromethane (DCM) were determined at 298 K and given values of ionic strength. Here, Kex± and Kex were expressed as [AgL﹢]o[Pic﹣]o/[Ag﹢][L]o[Pic﹣] and [AgLPic]o/[Ag﹢][L]o[Pic﹣], respectively: L symbolizes B15C5 or B18C6 and the subscript “o” denotes the organic phase composed of DCE or DCM. Individual distribution constants (KD,Pic) of picrate ion, Pic﹣, into the two diluents were also determined with the determination of Kex. From comparison of these KD,Pic values with those standardized, interfacial potential differences () at extraction equilibria were evaluated. Then, using these values, relations of the experimentally-determined logKex± or logKex values with their electrochemically-standardized ones were precisely discussed. Consequently, it was indicated that logKex± should be expressed as a function of .

Volatile components of Rhizoma Alpiniae Officinarum using three different extraction methods combined with gas chromatography-mass spectrometry

Volatile components from Rhizoma Alpiniae Officinarum were respectively extracted by three methods including hydrodistillation, headspace solid-phase microextraction （HS-SPME） and diethyl ether extraction. A total of 40 （hydrodistillation）, 32 （HS-SPME） and 37 （diethyl ether extraction） compounds were respectively identified by gas chromatography-mass spectrometry （GC/MS） and 22 compounds were overlapped, including β-farnesene, 7-muurolene, 2,6-dimethyl-6- （4-methyl-3-pentenyl）bicyclo[3.1.1]hept-2-ene, eucalyptol and cadina-1（10）, 4-diene and so forth, varying in relative contents. HS-SPME is fast, sample saving and solvent-free and it also can achieve similar profiles as those from hydrodistillation and solvent extraction. Therefore, it can be the priority for extracting volatile components from medicinal plants.

亚临界萃取和膜技术精制元宝枫籽油的工艺优化

为了提高元宝枫籽油(ASO)的质量特性和储藏稳定性,对亚临界萃取得到的元宝枫籽油进行精制,以去除磷脂、过氧化物和游离脂肪酸。本文对亚临界萃取ASO的提取工艺进行优化,并对得到的原油利用膜分离技术进行脱胶精制,以膜通量,脱胶率、碘值、过氧化值、酸价为指标,对不同孔径的陶瓷膜和不同截留分子量的聚醚砜膜进行筛选。考察膜截留分子量、温度和压力对膜通量的影响;通过响应面法,确定ASO精制的最佳工艺参数。同时采用气相色谱-质谱法比较精制前后脂肪酸的含量。结果表明,当粒径为30目、萃取温度50℃,固液比为1:4 g/mL,聚醚砜膜分子量为100 kD,温度44℃,压力1.9 MPa,ASO得油率均值为35.92%,脱胶率为86.73%,通量为12.51 L/m2·h,碘值为116.93 g/100 g,过氧化值为0.06 g/100 g,酸价为3.66 g/100 g,与原油相比脂肪酸含量无明显损失。研究结果显示,用膜分离法脱胶是一种提高油脂品质的有效手段,本研究可为优质元宝枫籽油的生产提供技术支持。

Application of the Electrochemical Method for Stripping Eu^（3＋） after Extraction with Benzo－15－crown－5 in Dichloromethane

Eu3+ is extracted at pH 6 with 5. 0×10-2 mol/L benzo-15-crown-5 in dichloromethane from 5. 0×10-2 mol/L aqueous solution of lithium picrate. The enriched extractability has been investigated. In a concentration range from 2. 4 ×10-4 to 1. 8 ×10-3 mol/L solution of europium nitrates, the enrichment coefficients are calculated with the phasc ratio (organic/aqueous) of 1: 5 or 4: 25. The ability of 0. 5 mol/L HNO3 as a back-extractant is discussed with the volume ratio [organic/(0. 5 mol/L HNO3)] of 1 : 3. Crown ether and picric acid exist in the back-extractivephase. Eu3+ is effectively separated from the organic phase by the electrochemical method. The separation efficiency is more than 84%. The optimum electrolysis time or cell voltage is obtained from the relation between the electrolysis current and the time or the voltage.

Insecticidal Activity of Crude Extracts of Hyptis suaveolens(Bush Mint)on Anopheles Mosquitoes Collected from Lafia,Nasarawa State,Nigeria

Anopheles gambiae is a vector that is responsible for the transmission of malaria parasites which causes high morbidity and mortality in Nigeria and the world at large.Human-vector contact can be reduced by the use of conventional repellents being sold in the market,though some of these repellent are not environmentally friendly and An.gambiae have developed resistance to some of these repellents.To this end,the phytochemical constituents and insecticidal activity of crude extracts of Hyptis suaveolens(bush mint)was determined on adult An.gambiae mosquitoes collected from Lafia,Nasarawa State,Nigeria to evaluate its effect in controlling them.Here,70%ethanolic and diethyl ether fat crude extracts were made from H.suaveolens dried leaves and used to carry out the experiment.The phytochemical screening of the ethanol extract revealed the presence of alkaloids,flavonoid,saponins,tannins,steroids and reducing sugar.Glycoside was not detected in the ethanol extract.Only steroids was detected in diethyl ether extract the rest of the phytochemical tested were absent.An.gambiae larvae were collected from the field and were raised to F1 progeny adults that were used for the study.WHO protocol for carrying out human bait repellency cage test was used.Human hand treated with the extracts was exposed to a cage containing 30 female mosquitoes for each of the extracts respectively.The ethanolic crude extract treatment proved to be more effective in repelling mosquitoes with 0%(0/30)mosquito landing than diethyl ether extract which had 40%(12/30)mosquitoes landing and the control hand(untreated left hand)had the highest landing rate 63.3%(19/30)which showed very high significant difference(χ^(2)=27.2619,df=2,P<0.00001)in relation to the treatments.After 24 hours holding period,the mortality rate of exposed mosquitoes was observed to be highest in the ethanolic treatment 73.3%(22/30).In conclusion,H.suaveolens extracts have repellency potential in controlling adult An.gambiae.

防风石油醚提取物调节中性粒细胞胞外诱捕网对类风湿性关节炎大鼠的改善作用及机制

目的 探究防风石油醚提取物通过调节中性粒细胞胞外诱捕网(NETs)对类风湿性关节炎(RA)大鼠的改善作用及机制。方法 采用牛Ⅱ型胶原与弗氏完全佐剂建立大鼠RA模型。将造模成功的大鼠随机分为模型组和防风石油醚提取物低、中、高剂量组(55、110、220 mg/kg),另设不造模的正常组,每组10只。各组大鼠灌胃相应药液或等体积2%吐温-80溶液,每天1次,连续28 d。观察大鼠足趾肿胀度并进行关节炎指数(AI)评分,检测大鼠血清中白细胞介素1β(IL-1β)、IL-10、IL-17、肿瘤坏死因子α(TNF-α)、25-羟基维生素D_3[25(OH)D_3]、髓过氧化物酶(MPO)、中性粒细胞弹性蛋白酶(NE)和NETs的水平,观察大鼠踝关节病理学形态变化,检测大鼠踝关节中瓜氨酸化组蛋白H3(CitH3)以及滑膜组织中细胞色素P450 24A1(CYP24A1)、细胞色素P45027B1(CYP27B1)、维生素D受体(VDR)、肽基精氨酸脱亚胺酶4(PAD4)的表达水平。结果 与模型组比较,防风石油醚提取物中、高剂量组大鼠给药后第14天至第28天的足趾肿胀度和AI评分均显著降低(P<0.05或P<0.01);血清中IL-1β、IL-17、TNF-α、MPO、NE和NETs水平均显著降低,IL-10、25(OH)D_3水平均显著升高(P<0.05或P<0.01);踝关节间隙变宽,结构明显改善;踝关节中CitH3以及滑膜组织中CYP24A1、PAD4表达水平均显著降低,滑膜组织中CYP27B1、VDR表达水平均显著升高(P<0.05或P<0.01)。结论 防风石油醚提取物可能通过调控维生素D系统,抑制NETs生成,进而改善RA症状。

鸦胆子石油醚提取物成分分析及降糖活性初探

目的:对鸦胆子石油醚提取物的主要成分进行分析,并对其降糖活性进行探讨。方法:采用石油醚萃取的方式提取鸦胆子,应用气相色谱-质谱联用技术(GC-MS)鉴定其成分,应用归一化法测定各成分的质量分数(相对含量)。色谱条件:色谱柱Agilent HP-5MS(30 m×250μm×0.25μm),流速1 mL/min,分流比15∶1,进样口温度300℃。程序升温条件:60℃保持5 min,以4℃/min升温至180℃,保持5 min,以2℃/min升温至280℃,保持10 min。质谱条件:离子源电子轰击(EI)源,离子源温度230℃,四级杆温度150℃,溶剂延迟3 min,电子能量70 eV,质荷比(m/z)范围50~900。数据库:NIST 08。降糖活性通过测试pNPG水解产物NPG的吸光计算而得。结果:从鸦胆子石油醚提取物成分中鉴定出脂肪酸、芳香酸、脂肪酸酯、醛、酮、萜、类固醇、烃类等53种成分,其中脂肪酸11种,脂肪酸酯20种,醛7种,烃9种,芳香酸1种,酮1种,萜1种,类固醇2种,生育酚1种。药理学研究表明,鸦胆子石油醚提取物具有α-葡萄糖苷酶抑制活性。结论:GC-MS能够高效准确快速鉴定鸦胆子石油醚提取物的化学成分,鸦胆子这一类成分的降血糖作用为进一步研究其作用机制奠定了基础。

一种新型的用于萃取铷的冠醚功能化磁性固相纳米材料

本研究成功制备了一种新型的用于萃取铷的冠醚功能化磁性固相纳米材料(CFE)。通过溶剂热法合成了Fe_(3)O_(4)纳米颗粒磁核,利用3-氨丙基三乙氧基硅烷在碱性环境下的酯水解反应,在磁核表面包覆SiO_(2)并修饰氨基,制备了Fe_(3)O_(4)@SiO_(2)-NH_(2)中间产物,再利用4′-羧基苯并-18-冠6-醚上的羧基与修饰在Fe_(3)O_(4)@SiO_(2)-NH_(2)表面的氨基在1-乙基-(3-二甲基氨基丙基)碳二亚胺盐酸盐的催化下发生酰胺化反应,将该冠醚修饰在中间产物的表面,制备了CFE新型材料。分析了Fe_(3)O_(4)、Fe_(3)O_(4)@SiO_(2)-NH_(2)、CFE的微观形貌、磁化性质、X射线衍射性质、红外吸收性质、元素组成,佐证了材料被成功制备,验证了CFE对Rb^(+)的萃取能力,研究了溶液pH对Rb^(+)萃取效果的影响。结果表明,室温下萃取30 min,在pH为13时CFE对Rb^(+)具有最佳的萃取效果,萃取率为90.0%。

DBC solvent extraction of U(VI) from thiocyanate medium

The extraction behavior of uranium(VI) from thiocyanate medium with dibenzo-18-crown-6 (DBC) in nitrobenzene and the effects of alkali canons on the extraction were investigated. The results showed that the uranium (VI) can be effectively extracted in the presence of potassium canon, uranium (VI) is extracted as complex anionic species UO2(SCN)2, and the stoichiometry of the extracted complex is KUO2(SCN)32DBC(o)’

Inhibitory Effect of Extracts from Helianthus tuberosus Leaves against Phytophthora capsici and Pot Verification Test

By growth rate method, the inhibitory effects of five solvent extracts from Helianthus tuberosus leaves against Phytophthora capsici were studied in the test. The results showed that different solvent extracts all had inhibitory effect against P. capsici, while 12.5 mg/mL of extracts from H. tuberosus leaves with petroleum ether and ethyl acetate as solvents had the highest inhibitory effect against P. capsici, reaching 100%. In case of various solvent extracts with different concentration gradients, ethyl acetate extract had the most significant inhibitory effect; when the concentration was 5 mg/mL, the inhibitory effect of ethyl acetate extract had reached 100% ; when the concentration reduced to 2.5 mg/mL, the inhibitory effect was still （27.91 ±2. 076） %, significantly higher than that of other solvent extracts at the same concentration. The 50 times dilution of ethyl acetate extract from H. tuberosus leaves was selected for pot test against pepper blight. , and the results showed that its control effect against pepper blight reached 100.00%, superior than that of chemical agent 25% metalaxyl WP 400 times dilution.

基于低场核磁共振的烤烟烟叶石油醚提取物含量检测方法

针对当前传统索氏提取法在烤烟烟叶石油醚提取物含量检测上存在的检测速度慢、操作繁琐、溶剂污染等问题,采用低场核磁共振法检测烟叶中石油醚提取物含量,优化烘干时间、样品质量、回波时间、重复扫描次数等参数,验证最优参数下检测方法的重复性和精密度,并与传统索氏提取法的检测结果进行对比。结果表明:将过40目筛的3.0 g烟叶粉末置于80℃烘干4 h,在回波时间0.25 ms和重复扫描次数8次的条件下进行石油醚提取物含量检测,检测结果良好,标准曲线R2达到0.99981,重复性的相对标准差为1.45%~2.99%,日内、日间精密度分别为2.61%、1.10%。低场核磁共振法与索氏提取法的石油醚提取物含量检测结果间的相关系数达0.99855,绝对误差为0.02%~0.35%,相对误差为0.26%~3.69%。相较于传统索氏提取法,低场核磁共振方法简单、快速、准确,且无溶剂污染,适用于大批量烟叶石油醚提取物的准确定量。

化州市不同结香方法沉香化学成分差异分析

为分析整树结香、自然结香和虫漏结香3种方式获得沉香化学成分的差异,评价不同结香方式的效果,对采自化州市平定镇的整树结香、自然结香、虫漏结香3种不同沉香样品采用乙醚超声浸提法制备乙醚浸出物,通过气相色谱质谱技术完成对浸出物的化学成分分析和鉴定工作。研究结果表明,不同结香样品乙醚浸出物含量在4.51%~14.23%之间,倍半萜类和色酮类化合物相对含量之和均超过70%,其中倍半萜类化合物数量介于19~26个,相对含量均超过50%,色酮类化合物数量介于2~7个,相对含量在2.09%~27.93%之间。与自然结香、虫漏结香等天然形成沉香相比,整树结香人工诱导技术可获得较高品质的沉香。

沙旋覆花石油醚部位洗脱组分的体外抗肿瘤活性研究

采用CCK-8法从沙旋覆花中筛选出具有抗肿瘤活性的石油醚部位洗脱组分,研究了其对人食管癌细胞Eca109增殖的抑制作用,并通过4′,6-二脒基-2-苯基吲哚(DAPI)染色法探究了其对Eca109细胞抑制作用的方式。结果表明,沙旋覆花石油醚部位洗脱组分(除23^(#)外)对Eca109细胞具有不同程度的抑制作用,其中71^(#)组分的抑制作用最强,对Eca109细胞的IC_(50)值为8.19μg·mL^(-1);沙旋覆花石油醚部位洗脱组分可通过诱导细胞裂亡和凋亡发挥抗食管癌作用,为后续开展旋覆花属植物抗食管癌活性成分筛选与药效评价奠定了基础。

榆干玉蕈子实体及其提取物的免疫调节作用

为研究榆干玉蕈(Hypsizygusulmarius)子实体粉末及提取物对小鼠的免疫调节作用,分别采用榆干玉蕈子实体粉末(高、低剂量分别为1.2、0.3g·kg^(-1))、石油醚提取物(高、低剂量分别为1.392、0.348mg·kg^(-1))、乙酸乙酯提取物(高、低剂量分别为3.306、0.826 mg·kg^(-1))、水提取物(高、低剂量分别为28.78、7.19 mg·kg^(-1))灌胃大黄水煎液建立的模型小鼠,测定其体质量、脾脏指数及血清中白细胞介素2(interleukin-2,IL-2)、白细胞介素6(interleukin-6,IL-6)、免疫球蛋白M(immunoglobulin M,IgM)、干扰素γ(interferon-γ,IFN-γ)、D-木糖(D-xylose)、白蛋白(albumin,ALB)、胰脂肪酶(pancrelipase,PL)含量,采用苏木素-伊红染色观察小鼠脾脏组织显微结构,采用RT-qPCR法检测维生素D结合蛋白(D binding protein,DBP)和紧密连接蛋白(occludin,OCLN)的基因表达情况,并采用Westernblotting方法检测DBP和OCLN蛋白表达情况。结果表明:与模型组相比,第14天,各给药组小鼠体质量均显著增加。粉末高剂量组脾脏指数显著增加。所有给药组D-xylose、IFN-γ、ALB、IL-2、IgM、PL含量均显著增加,IL-6含量显著降低。各给药高剂量组DBP基因相对表达量显著升高,所有低剂量组显著降低;粉末低剂量组、石油醚提取物高和低剂量组、水提物高和低剂量组的OCLN基因相对表达量均显著升高。各给药组DBP和OCLN的蛋白表达量均显著升高。榆干玉蕈子实体及各提取物均通过免疫调节发挥作用,研究结果可为榆干玉蕈进一步开发利用提供参考。

酸热法提取黑水虻鲜幼虫油脂工艺研究

【目的】构建黑水虻油脂的快速、高效的新型提取工艺,解决传统提取工艺中因乳化作用和细胞破碎不足导致油脂提取率较低的问题,为黑水虻油脂的提取及黑水虻油脂的规模化发展提供新思路。【方法】使用酸热法提取黑水虻鲜幼虫油脂,通过控制变量法选取黑水虻鲜幼虫油脂的预处理方法和提取溶剂,经单因素试验和正交试验对提取工艺进行优化,分析黑水虻鲜幼虫油脂的理化指标,并通过高效气相色谱仪分析其脂肪酸组成。【结果】酸热法提取黑水虻鲜幼虫油脂的最佳预处理方法为添加质量分数5.0%的柠檬酸溶液匀浆破碎(m(鲜幼虫/g)∶V(溶液/mL)=1∶1),最佳提取溶剂为石油醚,提取工艺条件为柠檬酸溶液质量分数5.0%、料液比m(鲜幼虫/g)∶V(石油醚/mL)=1∶5、提取时间60 min和提取温度50℃。在此条件下,油脂提取率达到94.67%,且耗时4 h便可得到黑水虻鲜幼虫油脂。黑水虻鲜幼虫油脂的酸值为9.30 mg·g-1,过氧化值为1.74 mmol·kg^(-1),皂化值为227.23 mg·g-1。鲜幼虫油脂共检测出20种脂肪酸,其中,亚油酸与月桂酸的含量最高,分别为32.72%和30.75%。【结论】酸热法能快速、高效地提取黑水虻鲜幼虫油脂,既节省了干燥成本,又保证了油脂的品质和脂肪酸组成。

基于谱效关系的地菍石油醚提取物抗炎活性物质基础研究

目的建立地菍石油醚提取物的指纹图谱,并结合细胞药效学实验探究其抗炎活性物质基础。方法采用高效液相色谱(HPLC)法,利用《中药色谱指纹图谱相似度评价系统(2012版)》生成20批地菍石油醚提取物的指纹图谱,并进行相似度评价和共有峰指认;建立脂多糖诱导的小鼠单核巨噬细胞RAW264.7炎症模型,以一氧化氮(NO)、肿瘤坏死因子α(TNF-α)的抑制率为指标,考察地菍石油醚提取物的抗炎活性,并运用灰色关联度法、偏最小二乘回归分析法进行谱效关系研究;采用分子对接验证抗炎活性成分与TNF-α、诱导型一氧化氮合酶(iNOS)蛋白质受体的结合活性。结果20批地菍石油醚提取物的指纹图谱中有19个共有峰,20批样品的相似度为0.603~0.990;指认了牡荆素(5号峰)、异牡荆素(6号峰)、鞣花酸(7号峰)、槲皮素(9号峰)、木犀草素(10号峰)5个成分。地菍石油醚提取物19个共有峰与NO、TNF-α抑制率的关联度均大于0.7,峰19、13、9(槲皮素)、12、5(牡荆素)、6(异牡荆素)、8、7(鞣花酸)、18、1与NO抑制率呈正相关;峰8、10(木犀草素)、13、15、3、19、17、7(鞣花酸)、18、1与TNF-α抑制率呈正相关。牡荆素、异牡荆素、槲皮素与iNOS蛋白质受体的结合能均小于-5.0 kcal/mol。结论牡荆素、异牡荆素、槲皮素可能是地菍石油醚提取物发挥抗炎作用的药效物质基础。

山慈菇的乙酸乙酯、石油醚、氯仿萃取物挥发性成分鉴定

目的鉴定山慈菇的乙酸乙酯、石油醚、氯仿萃取物中的挥发性成分。方法取3 kg山慈菇加工成粉末,分别以乙酸乙酯、石油醚、氯仿萃取,采用气相色谱—质谱联用法(GC-MS)对乙酸乙酯萃取物、石油醚萃取物、氯仿萃取物中挥发性成分进行分析与鉴定。结果山慈菇乙酸乙酯萃取物中共鉴定出51种化合物,以儿茶酚含量最高,其次是4-羟基苯甲醛、2-乙基-3-甲基吡嗪、Phenol,4-(ethoxymethyl)-、肉桂酸、间羟基苯甲酸等;山慈菇石油醚萃取物共鉴定出35种化合物,包括肉桂酸、棕榈酸丁酯、十七酸甲酯、油酸、亚油酸等;山慈菇氯仿萃取物共鉴定出28种化合物,包括Phenol,4-(ethoxymethyl)-、2,6-二甲氧基苯酚、2-乙基-3-甲基吡嗪、肉桂酸等。结论在山慈菇乙酸乙酯、石油醚、氯仿萃取物中抗癌挥发性成分都发现了肉桂酸,在山慈菇乙酸乙酯萃取物中发现了香草酸、间羟基苯甲酸、4-羟基苯甲醛等抗癌成分。山慈菇不同萃取物中首次发现儿茶酚、2-乙基-3-甲基吡嗪、Phenol,3-甲基环戊烷-1,2-二酮、甲基环戊烯醇酮、棕榈酸丁酯、十七酸甲酯、油酸、亚油酸、2,6-二甲氧基苯酚、2-乙基-3-甲基吡嗪等成分。

气相色谱-质谱法测定小麦粉中苯甲酸含量

建立了一种气相色谱-串联三重四级杆质谱的苯甲酸添加剂测定方法,并对该检测方法的参数进行了优化。试验结果表明:(1)当以酸性石油醚作为提取试剂时,在提取固液比为1∶8,超声提取时间为50 min条件下,苯甲酸的提取率最高;(2)在最优参数条件下,苯甲酸的检出限和定量限分别为0.5 mg/kg和1.5 mg/kg,在1~100μg/mL的浓度范围内表现出良好的线性关系,且相关系数R 2大于0.999;在1、10、20 mg/kg加标水平下,苯甲酸回收率在91.7%~107.6%范围内,其中在10 mg/kg加标水平下的相对标准偏差(RSD)为0.9%。综上,该检测方法简单、快捷和准确,可用于小麦粉中添加剂残留量的测定。