十二烷基苯磺酸钠和链烷醇酰胺复配体系中组分含量的测定

分别采用荧光光谱法和化学分析法测定复配溶液中的十二烷基苯磺酸钠(SDBS)和链烷醇酰胺的含量。在复配溶液中加入与SDBS等物质的量的β-环糊精,不仅能增强SDBS的荧光强度,还能显著降低烷醇酰胺对SDBS的干扰。采用荧光光谱法测定复配溶液中SDBS的含量,加标回收率在101%~102%之间。又在试样溶液中以硫酸作为催化剂,使其中的链烷醇酰胺水解,反应时间为10h,随后采用化学分析法测定复配溶液中烷醇酰胺含量,加标回收率在98.2%~98.9%之间。     

红外光谱法定量测定有机硅材料中的炔醇

利用含炔醇有机硅材料中醇的特征峰,建立了用傅立叶红外光谱法测定有机硅材料中炔醇含量的定量分析方法。以测定甲基硅油中加入的乙炔环己醇含量为例,对比了标准曲线法和标准加入法,标准加入法更适合基体复杂的试样的分析,准确度优于标准曲线法,其有效测量范围为0.04%~5%,回收率在98.2%~101%。对实际样品进行检测,结果 RSD=1.8%(n=3)。     

毛细管气相色谱法测定高纯度三十烷醇

正三十烷醇是一种新型植物生长激素。目前国内外已广泛研究和使用。但对三十烷醇产品定量分析还是值得研究的课题。 目前一般以蜂蜡为原料,经过皂化有机溶剂重结晶得到三十烷醇。定量分析多采用填充柱法,其分离效果较差,峰形不理想。我们改用甲基乙烯基     

宽叶独行菜石油醚部分非极性馏分GC-MS分析

为了研究宽叶独行菜石油醚洗脱部分的成分,采用气质联用技术首次测定了宽叶独行菜中石油醚洗脱部分的非极性馏分。结果表明正二十七烷(Heptacosane)含量最高达到35.214%,其次为正二十九烷(Nonacosane)含量为19.768%,正二十五烷(Pentacosane)10.448%,异构二十九烷2-methyl Octaco-sane7.848%异构二十七烷(2-methylHexacosane)5.886%和正二十八烷(Octaco-sane)2.507%。含量大于1的有正二十三烷(Tricosane),正二十四烷(Tetraco-sane),正二十六烷(Hexacosane),异构二十八烷(2-methylHeptacosane),反异构二十八烷(3-methylHeptacosane),反异构三十烷(3-methyl Nonacosane),异构三十一烷(2-methyl Triacontane)和正三十一烷(Hentriacontane)。     

一种新型植物生长调节剂—高纯度三十烷醇-1

早在1933年Chibnall等就首次从苜蓿中提取分离得到三十烷醇,又各蜂花醇。40多年后,Ries等指出苜蓿干草能促进农作物的生长并增加收成。。于是他们着手分离苜蓿中的活性组份,后经质谱鉴定,这种活性物质就是三十烷醇1。Ries认为三十烷醇-1是一种无毒,高效,快速及适用范围相当广泛的植物生长促进剂.一毫克样品就能使1000m~2(相当于     

烷基醇聚氧乙烯醚中二噁烷的测定

１引言随着现代工业的发展和人民生活水平的提高，家用洗涤剂的使用范围越来越广，使用量也在不断增加。烷基醇聚氧乙烯醚是液体洗涤剂的有效成份，其合成过程中产生的二噁烷是有害物质，虽其含量较低，但它能通过蒸气形式吸入人体，与眼、皮肤等接触，侵害人的肝、肾、皮肤、眼睛等多个部位，且能在人体内积蓄，给人们的健康造成危害。聚氧乙烯醚中二噁烷的测定尚未见报道。本文采用顶空气相色谱法对烷基醇聚氧乙烯醚中的二噁烷进行测定，选择了顶空条件，以保留值和加入已知物增加峰高法定性，外标法定量，建立了简便、准确、灵敏的分析测…     

库仑滴定法测定新洁尔灭溶液中溴化苄烷铵的含量

应用库仑滴定法测定了新洁尔灭溶液中溴化苄烷铵的含量。用0.09mol·L-1硝酸溶液和0.5%(w)明胶溶液以体积比10比1混合的混合溶液作电解液,银棒作阳极进行恒电流电解,电解电流为10mA。电解过程中,从银电极释放出的Ag+与试液中溴化苄烷铵的Br-反应生成沉淀。Br-被完全沉淀时,电流上升,滴定到达终点,根据法拉第定律计算溴化苄烷铵的含量。溴化苄烷铵的质量浓度在0.422 8~1.480g·L-1范围内与所消耗的电量之间呈线性关系。对同一样品的分析,本方法的测定结果与四苯硼钠滴定法的测定结果相符,本方法测定结果的相对标准偏差(n=6)为0.9%。用标准加入法进行回收试验,测得回收率在99.6%~102%之间。     

三相转移催化提取三十烷醇及其应用研究

三十烷醇-1(1-Triacontanol)又称蜂花醇，是一种新型的天然的植物生长调节剂，来源广、用量微、成本低、作用大、无公害。三十烷醇常与高级脂肪酸结合成酯，普遍存在于植物蜡和虫蜡中如蜂蜡、糠蜡、蔗蜡、棉蜡等，经皂化后分离提纯得到。其中由蜂蜡提取三十烷的关键是使其皂化，目前常     

水母雪莲提取物GC-MS分析

采用气质联用技术测定了水母雪莲提取物石油醚-丙酮(8∶2)部分,再用正已烷-乙酸乙酯(95∶5)洗脱部分的非烃酯化馏分。实验通过GC-MS法对水母雪莲提取物极性(非烃酯化馏分)进行了分析,其中共分离得到33个组分。采用面积归一化法测定了各组分的百分含量,并用气相色谱-质谱联用技术对其做了分析,结果表明,棕榈酸(Hexadecanoic acid)的含量很高,达39.71%。其次为亚油酸(9,12-Octadecadienoic acid)16.85%,油酸(9-Octadecenoic acid)10.29%,硬脂酸(Octadecanoic acid)5.90%。二甲氧基-十八烷酸的含量为4.23%,乌散烯(12)-酮(3)3.45%,浕-亚麻酸2.83%,三甲基十八烷酸2.80%,二十烷酸(花生酸)的含量为2.30%,β-香树精(β-Amyin)的含量为2.27%,羽扇醇1.33%。其中含量大于1的还有,二十二烷酸。     

Mn改性Ni/K/MoS2合成低碳醇催化剂反应性能研究

以不同的添加方式在Ni/K/MoS2催化剂中加入Mn助剂，考察其合成醇反应性能。结果表明，Mn/Ni/K/MoS2催化剂具有较好的合成低碳混合醇反应性能。共沉淀法以醋酸锰为前驱体加入0.6%的Mn助剂后，C2+含量，醇时空产率及选择性均明显提高;分步沉淀法使Mn的加入量增加到0.6%，醇时空产率明显增加。以浸渍法按化学计量加入Mn助剂考察其含量对催化剂合成醇性能的影响，当Mn/Mo（原子比）为1∶时，反应条件为315 ℃, 9.5 MPa, 6 000 h－1，醇时空产率和醇选择性分别达到最高值0.338?g/mL·h和69.6%。300 h的稳定性测试结果表明，共沉淀法改性的催化剂具有良好的稳定性。     

Three‐phase hollow fiber liquid‐phase microextraction combined with HPLC for determination of three trace acidic plant growth regulators in Anoectochilus roxburghii (Wall.) Lindl

The analysis of plant growth regulators presents a challenge due to their trace quantities and complex matrices. A novel, simple, and effective analytical method for the determination of three trace acidic plant growth regulators in Anoectochilus roxburghii (Wall.) Lindl was developed to address this issue. Three‐phase hollow fiber liquid‐phase microextraction combined with high‐performance liquid chromatography was applied for the enrichment, purification, and determination of three acidic plant growth regulators, namely, indole‐3‐acetic‐acid, indole‐3‐butyric‐acid, and (+)‐abscisic acid. The factors affecting extraction performance, including extractant species, pH of donor and acceptor phases, salt addition dosage, extraction time, temperature, and stirring rate, were investigated and optimized. Under optimum conditions, the proposed method provided good linearity (R², 0.9994–0.9999), low limit of detection (0.038–0.12 ng/mL), and acceptable relative recoveries (56.7–117.6%). The enrichment factors were between 153 and 328. The developed method was successfully applied to the enrichment and determination of plant growth regulators in Anoectochilus roxburghii (Wall.) Lindl and exhibited increased purification capacity, higher sensitivity, and decreased organic solvent consumption compared with conventional sample preparation methods. This method may provide a testing platform for the monitoring of plant growth regulator residues, ensuring the safe and effective use of traditional Chinese medicine.     

Derivatives of Some 2-Chloroethylphosphonic Acid Esters,with Plant Growth Regulating Activity

Abstract

A method for the synthesis of esters of 2-(dimethylsulfonium)ethylphos-phonic acid and the results of some trials showing the plant growth regulating activity of these compounds are presented. For the synthesis of the mentioned compounds, dimethyl sulphide is reacted with 2-chloroethylphosphonic acid esters; these esters are obtained through the complex[1] of AlCl₃, PCl₃ and 1,2-dichloroethan (1). Using the optimum reaction conditions, very good yields were obtained (96–99%). This complex is reacted with different alcohols to give 2-chloroethylphosphonic acid esters (2) (R?Me, Et, Pr, i-Pr, Bu, i-Bu, Pe). Using the optimum reaction conditions, in the case of methanol the maximum obtained yield was 50%. In the case of the other alcohols, the obtained yields were between 76 and 83%. An exception is i-propanol. whose ester was obtained with low yields and the reaction parameters modification have little influence on the yield. The reaction of the esters with dimethyl sulphide gives, in good yields (between 69 and 79%). esters of 2-(dimethylsulfonium)ethylphosphonic acid (3). substances with plant growth regulating activity.     

UPLC–MS–MS同时测定人参中4种植物生长调节剂残留量

建立超高效液相色谱–串联质谱法测定人参中4种植物生长调节剂残留的方法。样品以50%乙腈溶液室温振荡提取30 min,并采用分散固相萃取(DSPE)法净化,其中每毫升提取液加入50 mg C_(18)吸附剂,在优化后的仪器条件下进行测定。2,4-二氯苯氧乙酸、矮壮素、赤霉素、乙烯利分别在10~500,0.5~250,5~500,200~5 000μg/L范围内线性良好,相关系数r~20.99,检出限分别为7.5,0.4,4.0,150.0μg/kg,测定结果的相对标准偏差为3.05%~14.77%(n=6),加标回收率为69.6%~97.4%。该方法样品处理简单快速,检出限低,准确度和精密度高,适合于人参中2,4-二氯苯氧乙酸、矮壮素、赤霉素和乙烯利4种植物生长调节剂残留量的测定。     

高效液相色谱-串联质谱法测定果蔬中7种植物生长促进剂残留

建立了果蔬样品中对氯苯氧乙酸、赤霉酸(GA3)、2,4-二氯苯氧乙酸、α-萘乙酸、吲哚丁酸、6-苄氨基嘌呤、氯吡脲残留的高效液相色谱-串联质谱(HPLC-MS/MS)分析方法。样品用甲醇匀质提取2次,经Waters C18固相萃取小柱净化后,在高效液相色谱-串联质谱仪(HPLC-MS/MS)选择反应监测(SRM)模式下测定。采用质谱定性,外标法定量。色谱柱为Hypersil GOLD aQ(150 mm×2.1 mm,3μm)柱,以甲醇和水为流动相,梯度洗脱。果蔬样品在低、中、高3个加标水平下的平均回收率为79%～97%,相对标准偏差均不高于7.6%。7种植物生长促进剂在果蔬样品中的方法检出限为0.40～20.0μg/kg。该方法灵敏度高、操作简单,可作为大批量果蔬中植物生长促进剂残留的检测方法。     

Recent advances in application and progress of advanced materials as adsorbents in sample preparation for plant growth regulators

Plant growth regulators are a class of physiologically active substances that could modify or regulate basic physiological processes in the plant and defense against abiotic and biotic stresses, including natural plant growth regulators and synthetic ones. Different from natural plant growth regulators with low content and high cost of extraction in plants, synthetic ones can be produced in large-scale production and widely used in agriculture for increasing and securing yield and quality of the harvested produce. However, like pesticides, the abuse of plant growth regulators will have negative impacts on human beings. Therefore, it is important to monitor plant growth regulators residues. Due to the low concentration of plant growth regulators and complex matrices of food, it is necessary to isolate and extract plant growth regulators by appropriate adsorbents in sample preparation for obtaining satisfactory results. In the last decade, several advanced materials as adsorbents have shown superiority in sample preparation. This review briefly introduces the recent application and progress of advanced materials as adsorbents in sample preparation for extraction of plant growth regulators from the complex matrix. In the end, the challenge and outlook about the extraction of plant growth regulators of these advanced adsorbents in sample preparation are presented.     

DES-Fe3O4 composite for rapid extraction of residual plant growth regulators in edible vegetable oil

DES-Fe₃O₄ composite achieved a good performance on rapid extraction of residual plant growth regulators in edible vegetable oil with the help of external magnetic field.     

A Method for Evaluation of UV and Biologically Effective Exposures to Plants

This paper presents a method for evaluating the UV and biologically effective exposures to a plant canopy during the irradiation of soybean with supplemental levels of UV radiation in a greenhouse study. The method employs four materials as dosimeters that allow evaluation of the UV spectra. The exposures evaluated at three growth stages were less by factors of 0.44, 0.49 and 0.56 compared to the ambient exposures. At the end of the irradiation period, the ambient biologically effective exposure for generalized plant response was higher by 180% compared to that calculated over the canopy. This is the magnitude of the error in UV studies that provide the ambient exposure as a measure of the UV incident on the plant. Additionally, the difference between the ambient and canopy exposures varied during the growth stages. These results indicate that the dosimetric technique applied to evaluating the UV exposures over a plant canopy is a more accurate representation of the UV exposure incidence on a plant than any obtained by measuring the ambient exposures only.     

梯度洗脱高效液相色谱法测定红花玉兰中4种植物激素

建立了梯度洗脱高效液相色谱法测定红花玉兰中赤霉素(GA3)、生长素(IAA)、脱落酸(ABA)和玉米素(ZT)等4种植物激素的方法。采用Agilent ZORBAX SB-C18柱和紫外检测器,以甲醇和0.1 mol/L乙酸作为流动相进行梯度洗脱,流速1 mL/min,进样量10μL。GA3,IAA和ABA的检测波长为254 nm,柱温35℃;ZT的检测波长为270 nm,柱温40℃。采用外标法进行定量测定,4种植物激素的相关系数均大于0.9990。4种激素的回收率为98.1%~125.2%,相对标准偏差为0.31%~0.92%,日内和日间精密度RSD均<10%。方法可适用于红花玉兰多种组织的植物激素测定,为红花玉兰生长发育特性的研究奠定了基础。     

磁性Fe3O4亚微米球固相萃取-HPLC检测水中植物生长调节剂残留

建立了水中2,4-二氯苯氧乙酸(2,4-D)、萘乙酸(NAA)和6-芐基腺嘌呤(6-BA)3种植物生长调节剂残留分析的高效液相色谱方法.采用溶剂热还原法,以乙二醇和FeCl3·6H2O作原料,合成出形貌均一、分散性好、稳定性佳的磁性Fe3O4亚微米球,作为固相萃取材料,以静电吸附作用可以富集水中残留的2,4-D、NAA、6-BA 3种植物生长调节剂.水样经调节pH值和固相萃取净化后,高效液相色谱法测定.3种植物生长调节剂在0.1 ～10 mg/L范围内响应和浓度的线性关系良好,相关系数均大于0.999;2,4-D、NAA、6-BA的检测限分别为0.06、0.02、0.04 mg/L.在测定的自来水、河水和湖水3种水样中,添加回收率范围为73.20％ ～87.21％,相对标准偏差为1.11％ ～7.52％(n=3),为水中的2,4-D、NAA和6-BA残留监控提供了简单、快速、准确的测定方法.     

复合硝基酚钠盐的胶束电动力学毛细管色谱分析

本文在自行研制的高效毛细管电泳仪上建立了复合硝基酚钠盐的胶束电动力学毛细管色谱分析方法。用５０ｍｍｏｌ／Ｌ十二烷基硫酸钠、ｐＨ＝９．０的硼酸盐缓冲溶液，在２０ｋＶ电压下分离了５－硝基愈创木酚钠、对硝基酚钠、邻硝基酚钠，此法用于Ａｔｏｎｉｋ型植物生长调节剂的定量分析，相对偏差小于２％，回收率在１０１％￣１０５％之间。