高效液相色谱-质谱法测定大豆中磺酰脲类除草剂多残留量的研究

建立了高效液相色谱-质谱联用(HPLC-US)选择离子监测(SIR)同时检测大豆中10种磺酰脲类除草剂多残留量的方法。样品经乙腈提取,正己烷液-液分配,弗罗里硅土填充柱净化,然后采用HPLC-ESI( )-MS测定。对液-质分离、样品前处理条件进行了详细的研究和优化。10种磺酰脲类除草剂在25-1000μg/L范围内线性良好,相关系数为0．9996-0．9997。在0．02-1．0mg／kg浓度范围内,平均加标回收率在72．1％-98．8％之间,相对标准偏差为0．90％-7．74％。该方法简便、快速、灵敏,净化效果较好,可同时满足进、出口大豆中多种除草剂残留量的检验工作需要。     

固相萃取-高效液相色谱-质谱联机在线分析水中痕量除草剂

建立了饮用水中痕量除草剂的SPE－LC－MS联机测试方法,该方法仅用45min就可完成水样中7种除草剂（阿特法津,西草净,西码净,杀草净,敌稗,乙草胺,甲磺隆）的分析,检测限低于欧共体所要求的饮用水标准（单种农药浓度小于0．1ug/L）。比起液液萃取,离线SPE等其他前处理方法,在线SPE的结果的重现性和精密度方面大大优于前者,环境水样分析时间大大减少（所需时间为液液萃取的、1／60,离线SPE的1／20）,而且更安全性和可靠。我们已在华北某地的地表水和地下水中检测出阿特拉津（1．9ug/L)和乙草胺（1．64ug/L）。     

固相萃取/高效液相色谱法测定地表水中磺酰脲类农药的研究

建立了固相萃取/高效液相色谱法(SPE/HPLC)同时测定地表水中五种磺酰脲类农药的方法。研究了固相萃取提取、净化方法,优化了高效液相色谱条件并用二极管阵列检测器进行定量分析。五种磺酰脲类农药在0.1~10.0μg/mL范围内线性良好,相关系数在0.9992~0.9998之间,相对标准偏差在1.8%~4.1%之间,平均回收率为72.8%~103%。本方法中五种磺酰脲类农药的检出限在0.02~0.22 ng/mL范围。用该法分析了某水域地表水,取得满意结果,表明本方法具有一定的实用性。     

Simultaneous Determination of Major Constituents of Honeybee Venom by LC-DAD

The aim of the study was to develop an LC method for honeybee venom analysis, using cytochrome c as an internal standard. The SynChropack C8 6.5 μm, 4.6 × 100 mm column was applied. The bee venom was separated by linear gradient 5–80% B at 30 min (eluent A—0.1% TFA in water, eluent B—0.1% TFA in acetonitrile:water (80:20)). The flow rate of mobile phase was maintained at 1 mL min⁻¹, injection volume: 40 μL, separation temperature: 25 °C. The analysis was monitored at 220 nm. Several honeybee venom constituents were separated and the content of four of them (apamine, mast cell degranulating peptide, phospholipase A₂ and melittin) were determined. By applying this methodology differences in chemical composition of honeybee venom were evaluated. In order to confirm the data obtained, the following steps and parameters were taken into account for the validation of the method: selectivity, precision (injection repeatability, analysis repeatability), accuracy (recovery), linearity and operating range, limit of detection and limit of quantitation. All steps of validation proved that the developed analytical procedure was suitable for its intended purpose (standardization). Due to its simplicity, the developed method can be easily automated and incorporated into routine operations both in the bee venom identification, quality control and assay tests.

     

Simultaneous Determination of Major Constituents of Honeybee Venom by LC-DAD

The aim of the study was to develop an LC method for honeybee venom analysis, using cytochrome c as an internal standard. The SynChropack C8 6.5 μm, 4.6 × 100 mm column was applied. The bee venom was separated by linear gradient 5–80% B at 30 min (eluent A—0.1% TFA in water, eluent B—0.1% TFA in acetonitrile:water (80:20)). The flow rate of mobile phase was maintained at 1 mL min⁻¹, injection volume: 40 μL, separation temperature: 25 °C. The analysis was monitored at 220 nm. Several honeybee venom constituents were separated and the content of four of them (apamine, mast cell degranulating peptide, phospholipase A₂ and melittin) were determined. By applying this methodology differences in chemical composition of honeybee venom were evaluated. In order to confirm the data obtained, the following steps and parameters were taken into account for the validation of the method: selectivity, precision (injection repeatability, analysis repeatability), accuracy (recovery), linearity and operating range, limit of detection and limit of quantitation. All steps of validation proved that the developed analytical procedure was suitable for its intended purpose (standardization). Due to its simplicity, the developed method can be easily automated and incorporated into routine operations both in the bee venom identification, quality control and assay tests.     

磺酰脲类除草剂残留检测技术及其研究进展

磺酰脲类除草剂具有高效、低毒、低残留等特点,已经成为当前使用量最大的一类除草剂.随着该类除草剂在农业生产中的广泛使用,其残留问题以及对后茬作物产生的危害已经引起关注.由于磺酰脲类除草剂在环境和生物样品中痕量存在,且其化学和热不稳定,酸性条件下易水解,以及最大残留限量值日益严格,使其残留分析成为一项极具挑战性的工作.该文综述了近年来磺酰脲类除草剂残留分析的前处理方法和检测技术的研究进展,并详细介绍了分子印迹技术、在线联用技术和液相色谱-串联质谱技术在该类除草剂检测中的应用及其前景,为今后分析检测各类样品基质中磺酰脲类除草剂的残留提供参考和依据.     

Simultaneous Determination of Major Constituents of Honeybee Venom by LC-DAD

The aim of the study was to develop an LC method for honeybee venom analysis, using cytochrome c as an internal standard. The SynChropack C8 6.5 μm, 4.6 × 100 mm column was applied. The bee venom was separated by linear gradient 5–80% B at 30 min (eluent A—0.1% TFA in water, eluent B—0.1% TFA in acetonitrile:water (80:20)). The flow rate of mobile phase was maintained at 1 mL min^?1, injection volume: 40 μL, separation temperature: 25 °C. The analysis was monitored at 220 nm. Several honeybee venom constituents were separated and the content of four of them (apamine, mast cell degranulating peptide, phospholipase A₂ and melittin) were determined. By applying this methodology differences in chemical composition of honeybee venom were evaluated. In order to confirm the data obtained, the following steps and parameters were taken into account for the validation of the method: selectivity, precision (injection repeatability, analysis repeatability), accuracy (recovery), linearity and operating range, limit of detection and limit of quantitation. All steps of validation proved that the developed analytical procedure was suitable for its intended purpose (standardization). Due to its simplicity, the developed method can be easily automated and incorporated into routine operations both in the bee venom identification, quality control and assay tests.     

固相萃取/超高效液相色谱-串联质谱法测定化妆品中12种合成着色剂

建立了固相萃取/超高效液相色谱-串联质谱法(SPE/UPLC-MS/MS)同时测定指甲油、眼影、唇膏等化妆品中12种合成着色剂(酸性紫49、颜料红57、颜料红53∶1、酸性黄36、结晶紫、罗丹明B、分散黄3、颜料橙5、苏丹红Ⅰ、苏丹红Ⅱ、苏丹红Ⅳ和溶剂蓝35)的分析方法。样品用四氢呋喃(THF)、二甲基亚砜(DMSO)和甲醇分步超声波辅助萃取,HLB固相萃取柱净化后,在Acquity UPLC BEH-C18(2.1 mm×50mm,1.7μm)色谱柱上分离,乙腈和0.05%甲酸溶液为流动相梯度洗脱,采用多反应监测(MRM)模式进行检测,基质外标法定量。结果表明:12种着色剂在6 min内均显示较好峰形,其线性范围为0.5~800μg·L-1,相关系数均大于0.99。定量下限(LOQ,S/N10)为1.4~2 000μg·kg-1。在指甲油、眼影和唇膏中分别添加0.025~20 mg·kg-1浓度的着色剂进行加标回收实验,测定回收率为60.8%~118.0%,相对标准偏差(RSD)为2.3%~10.8%。该方法快速、简便、灵敏,适用于油状、粉状及膏状化妆品中禁限用着色剂的定量和确证分析。     

固相膜萃取/高效液相色谱法测定环境水体中的磺酰脲类除草剂

建立了一种基于C₁₈固相萃取膜预富集、高效液相色谱法定量分析环境水体中6种痕量磺酰脲类除草剂的快速分析方法。优化了色谱分离条件,考察了洗脱剂种类与体积、水样pH值和盐效应等条件对萃取效率的影响。在优化条件下,6种磺酰脲类除草剂的峰面积与其质量浓度呈良好的线性关系,苯磺隆的线性范围为0.10²0.0μg/L,其余均为0.05²0μg/L,相关系数为0.999 0⁰.999 5,方法检出限为0.019⁰.037μg/L。对地表水和海水的加标回收率分别为92.6%¹05.7%和89.8%¹08.7%,相对标准偏差分别为0.7%⁷.1%和0.5%⁴.0%。该方法操作简单、快速、准确、灵敏度高。     

Separation of Sulfonylurea Herbicides and Determination of Bensulfuron-methyl Residues in Tapwater by HPTLC

JPC – Journal of Planar Chromatography – Modern TLC - In this work we have studied the separation of a mixture of the sulfonylurea herbicides (metsulfuron-methyl, chlorsulfuron,...     

离子色谱法同时测定饮用水中5种消毒剂副产物

建立了离子色谱电导检测大体积进样同时测定饮用水中5种消毒剂副产物(亚氯酸盐、溴酸盐、氯酸盐、二氯乙酸和三氯乙酸)的方法.选用大容量IonPac AS19阴离子交换分析柱,以KOH溶液梯度淋洗,流速为1.0 mL/min,可在33 min内一次进样同时分析上述5种消毒剂副产物和7种常见阴离子.亚氯酸盐、溴酸盐、氯酸盐、二氯乙酸和三氯乙酸的检出限分别为0.43、0.68、0.78、1.04和1.53μg/L(500 μL进样),线性相关系数r＞0.9995.运用该法测定了自来水中5种消毒剂副产物,并对样品加标回收,回收率在97.6%～105.6%之间.对影响分离和测定的因素,如温度、共存非测定离子、相邻离子间等进行了研究.     

离子色谱法同时测定饮用水中11种无机阴离子

建立了饮用水中11种无机阴离子的离子色谱测定法。采用ISC–2100型离子色谱仪测定饮用水中的F–,S2–,Br O3–,Cl–,NO2–,NO3–,Cl O2–,Cl O3–,I–,SO42–,PO43–11种无机阴离子。水样过0.22μm滤膜后,经Ion Pac AS19离子色谱柱分离,用KOH溶液梯度洗脱,流量为1.0 m L/min,电导检测器检测,外标法定量。11种阴离子的质量浓度与色谱峰面积在测定范围内呈良好的线性关系(r≥0.999 2),检出限为0.000 7~0.005 mg/L,相对标准偏差为0.2%~4.9%(n=6),加标回收率为87.0%~104.8%。方法简便、快速,精密度和准确度高,适合于饮用水中11种无机阴离子的同时测定。     

SPE/GC-MS/SIM法同时测定水中7类27种SVOCs的方法研究

通过优选色谱柱,进一步改进色谱分离条件,优化前处理方法,建立了一种快速、高效测定水中7类27种半挥发性有机污染物(SVOCs)的GC-MS方法。该法可分析的目标物种类多、前处理速度快、萃取溶剂用量少、环境污染小、色谱运行时间短,40 min内完成分析,适用于大批量样品检测。另外,使用基质匹配标准溶液配制标准曲线,减小了基质效应,采用分段法选择离子(SIM)扫描,可获取更高灵敏度。该方法的检出限为0.000 4~0.013μg/L,回收率为70.5%~92.8%,相对标准偏差(RSD,n=6)不大于11.2%。     

高效液相色谱法同时测定大豆中12种酰胺类除草剂的残留量

建立了大豆中12种酰胺类除草剂多残留量同时检测的高效液相色谱方法。样品经丙酮提取、弗罗里硅土柱净化后,用高效液相色谱-二极管阵列检测器检测。在0.05～1.0 mg/kg的添加水平范围内,12种酰胺类药物的回收率为75%～102%,相对标准偏差为1.9%～16.1%；12种酰胺类除草剂的测定低限均能达到国家相关的残留限量要求。对样品的前处理条件进行了研究和优化,经商品化的固相萃取柱净化过的样品干扰杂质较少,有利于后续的检测分析和方法的推广应用。该方法能够在35 min内完成一次分析,具有快速、灵敏、准确、可靠的特点。     

高效液相色谱-质谱联用法测定茶叶中30种磺酰脲类除草剂的残留量

提出了高效液相色谱-质谱联用法测定茶叶中30种磺酰脲类除草剂残留量的方法。样品经少量水浸泡后乙腈提取,经Cleanert HXN固相萃取柱净化,用乙腈与0.02mol·L-1磷酸溶液(按体积比9比1混合)的混合液洗脱,洗脱液经氮气吹干后用1mL流动相溶液溶解残渣,所得溶液供高效液相色谱-质谱分析,用外标法定量。30种磺酰脲类标准品的质量浓度在100μg.L-1以内呈线性,方法的检出限(2S/N)在2～10μg.kg-1之间。平均加标回收率在74.5%～115.5%之间,相对标准偏差(n=6)在1.30%～9.36%之间。     

Simultaneous Determination of Six Major Constituents in the Stems of Kadsura heteroclita by LC-DAD

The stem of Kadsura heteroclita is a traditional Chinese medicine with a variety of biological activities. For efficient monitoring of the quality of the herb, a simple, rapid, and accurate HPLC method has been developed for simultaneous determination of five cyclolanostane triterpenoid compounds (schisanlactone E, nigranoic acid, schisandronic acid, and heteroclitalactones A and D) and one tetrahydrofuran lignan (d-epigalbacin) in the stems of K. heteroclita. These six compounds were separated on a C₁₈ column by elution with a mobile-phase gradient prepared from acetonitrile and 0.05% (v/v) aqueous phosphoric acid. The flow rate was 1.0 mL min⁻¹ and the detection wavelength was 210 nm. The recovery of the method was in the range 95.03–102.19% and a good linear relationship (r ² > 0.9999) was obtained between response and compound concentration over a relatively wide range. The method was successfully applied to analysis of the herb collected at different stages of growth.     

Determination of Herbicides of the Chlorophenoxycarboxylic Acid Type in Natural and Drinking Water by Capillary Zone Electrophoresis

The method of capillary electrophoresis was applied to separate and quantitatively determine herbicides belonging to the class of chlorophenoxycarboxylic acids: 2,4-dichlorophenoxyoleic, 2,4-dichlorophenoxypropionic, 2,4,5-trichlorophenoxyacetic, 2,4-dichlorophenoxyacetic, and phenoxyacetic, and the final product of their decomposition in an aqueous medium of 2,4-dichlorophenol. The influence exerted by - and - cyclodextrin on the selectivity of the separation system under study was analyzed. The hindering effect of humic acids on the separation and determination of phenoxycarboxylic acids by capillary electrophoresis was assessed.     

事蔬菜中残留三嗪农药的检测

建立了同时检测西红柿中11种三嗪除草剂残留量的高效液相色谱-紫外检测-质谱定性法.样品经纯水-甲醇提取,C12固相萃取柱净化,然后采用高效液相/紫外/质谱检测法测定,液相外标法定量.对样品前处理和色谱条件进行了研究和优化.11种三嗪除草剂在0.02×10-6～1.0×10-6 g/mL范围内的线性良好,相关系数为0.998 7～0.999 9,在0.01～0.1μg/g范围内,平均添加回收率在72.1%～101.0%,相对标准偏差为1.2%～5.1%.方法简便、快速、净化效果好.     

Application of SPE Using Multi-Walled Carbon Nanotubes as Adsorbent and Rapid Resolution LC-MS-MS for the Simultaneous Determination of 11 Triazine Herbicides Residues in River Water

A method for the simultaneous determination of 11 triazine herbicides residues in river water has been developed. It involves solid-phase extraction (SPE) pretreatment step and rapid resolution liquid chromatography-tandem mass spectrometry (RRLC-MS-MS). In the SPE pretreatment step, the adsorptive performance of MWCNTs material as SPE adsorbent and the elution capability of five kinds of solvents were investigated; in the LC separation step, a rapid resolution high throughput LC column, was used and the gradient elution mode adopted. The linear correlation coefficients (r ²) of the method for 11 target analytes varied between 0.9930 and 0.9980, the mean recoveries were in the range of 73.0 and 98.0% with relative standard deviations (RSD) 2.6 ~ 4.2%, the method detection limits (MDL) were all below 0.1 ng L^?1. An expanded uncertainty of not more than 20% was estimated for each analyte at the spiked concentration of 4.0 μg L^?1. The proposed method was applied to the determination of the residue concentrations of 11 pollutants in Songhuajiang River water.     

同时测定水中阴、阳离子的单柱阴离子排斥-阳离子交换色谱法

采用单柱离子色谱系统和电导检测的方法,以丙二酸为淋洗液,同时有效地分离、检测了溶液中SO42-、Cl -、NO3-、F -、Na 、NH4 、K 、Mg2 、Ca2 9种离子。研究了丙二酸浓度和流速对各离子保留时间及电导检测行为的影响。该法用于目前市售饮用水中的阴阳离子分析 ,得到满意的结果