两种样品处理方法对LC-MS/MS测定鸡肉中金刚烷胺基质效应比较

比较了液液萃取结合分散固相萃取(QuEChERS)和Oasis MCX小柱固相萃取(SPE)提取两种样品处理方法,分析鸡肉中金刚烷胺的基质效应。从绝对基质效应、提取回收率、方法过程效率及方法稳定性等方面的考察发现,经QuEChERS法和SPE法两种前处理方法处理后,不同浓度金刚烷胺的绝对基质效应均大于90%。SPE法虽能增强金刚烷胺的离子化效率,但金刚烷胺的提取回收率小于85%,方法过程效率也很低。与之相比,采用QuEChERS法处理鸡肉样品后,不仅能够有效增强金刚烷胺离子化效率,同时提取回收率和方法过程效率也相对较高且稳定,更适合作为鸡肉中金刚烷胺检测的前处理方法。     

HLB固相萃取小柱同时萃取水样中10种优先控制有机污染物

固相萃取(SPE)技术是有机分析的常用前处理方法,新型亲水/亲油平衡(HLB)基质反向填料小柱是适用于大多数有机污染物前处理的广谱性SPE小柱。利用HLB固相萃取小柱同时对国标要求优先控制的10种有机污染物进行批量富集前处理,再采用高效液相色谱(HPLC)外标检测方法检测了重庆主城区长江沿岸某水厂进出水和管网水中10种有机污染物的浓度。10种有机污染物在该方法中的定量检测限范围为0.100~0.500μg·L~(-1),精密度RSD0.30%(n=7),重复性RSD15%(n=7),加标回收率范围为71.0%~93.6%,满足国标检测要求。同时,HLB固相萃取小柱将10种目标有机物的前处理时间从40h缩短为8h,极大提高了检测效率。     

高效液相色谱法同时测定土壤中毒死蜱残留及其有毒代谢物3,5,6-TCP

通过对色谱分离条件优化、提取体系建立和固相色谱小柱筛选,建立了用弗罗里硅土固相萃取小柱净化高效液相色谱法同时测定土壤中毒死蜱农药残留及其有毒代谢物3,5,6-TCP.方法加标回收率在59％～87％之间,检测限为0.0005～0.03 μg/g,日内回收率标准偏差RSD≤4.3％,日间回收率标准偏差RSD≤4.9％,方法...     

液液提取-固相萃取-气相色谱法测定牛肉中蝇毒磷残留量的研究

建立了液液提取-固相萃取-气相色谱火焰光度法(LLE-SPE-GC-FPD)测定牛肉中蝇毒磷的残留量.优化了气相色谱分离条件,研究了样品基质对蝇毒磷测定的影响,考察了Florisil固相萃取小柱和ODS固相萃取小柱的萃取效果,并选择乙酸乙酯为洗脱剂,考察了液-液提取和固相萃取的回收率.将该方法用于牛肉中蝇毒磷的测定,其检出限为0.02 μg/mL,回收率高于83%,相对标准偏差13.7%.使用气相色谱质谱仪(GC-MS)对样品中的蝇毒磷进行定性分析,其特征离子和相对丰度为362(100)、226(55)和210(40).     

全自动固相萃取技术同时测定动物产品中9种磺胺药物残留

针对目前动物产品中兽药残留检测样品前处理繁琐的问题,应用全自动固相萃取技术对动物产品中9种磺胺类药物残留检测的样品前处理方法进行了系统的研究,对提取溶剂、固相萃取柱、淋洗液、洗脱溶剂及仪器分析条件进行了优化选择,建立了新型磺胺药物残留检测的全自动固相萃取净化方法.经不同检测单位验证,该方法的加标回收率为78.4%～107.8%,精密度为3.9%～11.0%检出限为0.010～0.020mg/kg,满足出口检测要求.     

固相萃取-GC/MS法测定水样中20种有机氯农药

建立了用固相萃取小柱提取和净化、GC/MS定性定量同时测定水样中20种有机氯农药的方法。方法采用OasisHLB固相萃取小柱萃取富集水样,二氯甲烷洗脱,加入菲-d₁₀作为内标,利用GC/MS进行定性定量,步骤简便,线性响应良好,干扰小,方法检出限为0.21～0.72 ng/L（按水样1L计）,加标回收率为64.8%～122%,RSD为1.2%～11.0 %。成功利用该方法对广西实际河水样品进行了检测。结果表明方法可以同时满足环境水样中20种痕量有机氯农药的测定。     

气相色谱-质谱法测定含油污泥中16种多环芳烃

采用超声提取和固相萃取小柱净化的前处理方法,结合气相色谱-质谱法(GCMS),建立了含油污泥中16种多环芳烃的检测方法。以新疆的油田采油或钻井等过程中产生的含油污泥为样品,经超声提取,固相萃取(SPE)小柱除杂净化后,用GC-MS法进行定量分析。16种多环芳烃在0.005~0.200mg/L范围内线性关系良好,相关系数为0.998~0.999,检出限(S/N=3)在0.26~2.38μg/kg之间,以0.200、0.500和1.000mg/L添加浓度水平进行方法学验证,回收率在60.20%~149.66%范围内,相对标准偏差为3.37%~16.84%。该方法具有快速、简便、灵敏度高等特点,能满足含油污泥中16种多环芳烃的检测要求。     

茶叶中有机氯和拟除虫菊酯多种农药残留同时分析的样品前处理研究

建立了茶叶中同时分析12种有机氯和拟除虫菊酯类农药残留的样品提取和固相萃取(SPE)前处理方法.试样在超声条件下用正己烷提取后用自制弗罗里圭(florisil)/石墨化碳复合固相萃取小柱净化,然后采用气相色谱-电子捕获检测器(GC-ECD)测定.研究结果表明,当茶叶中农药加标在4.93～201.00 ng/g范围内时,添加回收率为68.9%～112.2%,相对标准偏差为2.43%～15.8%,方法的检出限范围在2.52～10.59 ng/g.     

高效液相色谱法同时检测乳制品中3种β-内酰胺酶抑制剂的残留量

建立了乳制品中3种β-内酰胺酶抑制剂克拉维酸钾、他唑巴坦和舒巴坦的提取和固相萃取净化方法。样品经水溶后,用丙酮沉淀蛋白质。上清液在弱酸性条件下用PWAX固相萃取小柱(60 mg/3 mL)富集、净化,0.05%(如无特殊说明均为体积分数)氨水-甲醇溶液洗脱。然后采用高效液相色谱-二极管阵列检测器(HPLC-PAD)分离检测。分析柱为资生堂CAPCELL PAK MG-C18(150 mm×4.6 mm,5μm);流动相为0.03%磷酸-乙腈。该方法对克拉维酸钾、他唑巴坦和舒巴坦的最低检测质量浓度均为0.03 mg/L;纯牛奶、酸奶和奶粉中的回收率在84.6%~101.7%之间,RSD在2.2%~7.4%之间(n=6);在0.05~5 mg/L范围内均呈良好的线性关系,线性回归系数r>0.999。该方法的前处理净化效果好、检测灵敏度高、回收率和重现性良好,适用于乳制品中β-内酰胺酶抑制剂的测定。     

高效液相色谱法检测畜禽肉中四环素类药物残留的条件优化

对畜禽肉中四环素类残留的检测方法进行改进,选用Na2EDTA-McIlvaine缓冲溶液作为提取液进行超声提取,经C18固相萃取小柱净化,脱溶剂后用流动相三氟乙酸-乙腈溶解,使用高效液相色谱-PDA检测器分段采集355 nm及270 nm波长下的色谱信息,对前处理方法及色谱条件进行优化。四环素、土霉素在0.01～1μg/g范围内,金霉素、多西环素在0.02～2μg/g范围内回收率为60%～85%,相对标准偏差小于5%,可以满足国家残留限量0.1～0.6μg/g的检测要求。     

Use of inverse gas chromatography to determine thermodynamic parameters of aroma-starch interactions

A new instrumental setup for automated extraction of solid samples by online coupling of pressurized liquid extraction, automated SPE (solid-phase extraction) and HPLC is presented. From the extraction to the chromatogram no manual sample handling is required. The application to the determination of proanthocyanidins in malt reduces time and manual work to a minimum compared to former manual methods. Twenty samples can be processed within 24 h in respect to eight samples with the manual method. Using the features of the instrumental coupling, an optimized strategy for SPE of proanthocyanidins from natural samples was developed, requiring no evaporation step, using commercial cartridges and delivering concentrated eluates. The recovery of five main malt proanthocyanidins was 97%, with a reproducibility of 5%. This new instrumental coupling is thought to reduce time and costs along with improved results for a broad range of solid sample materials.     

Bamboo charcoal as adsorbent for SPE coupled with monolithic column-HPLC for rapid determination of 16 polycyclic aromatic hydrocarbons in water samples

The coupling of solid-phase extraction (SPE) using bamboo charcoal (BC) as an adsorbent with a monolithic column-high performance liquid chromatography (MC-HPLC) method was developed for the high-efficiency enrichment and rapid determination of 16 polycyclic aromatic hydrocarbons (PAHs) in water. Key influence factors, such as the type and the volume of the elution solvent, and the flow rate and the volume of the sample loading, were optimized to obtain a high SPE recovery and extraction efficiency. BC as an SPE adsorbent presented a high extraction efficiency due to its large specific surface area and high adsorption capacity; MC as an HPLC column accelerated the separation within 8 min because of its high porosity, fast mass transfer, and low-pressure resistance. The calibration curves for the PAHs extracted were linear in the range of 0.2-15 μg/L, with the correlation coefficients (r(2)) between 0.9970-0.9999. This method attained good precisions (relative standard deviation, RSD) from 3.5 to 10.9% for the standard PAHs I aqueous solutions at 5 μg/L; the method recoveries ranged in 52.6-121.6% for real spiked river water samples with 0.4 and 4 μg/L. The limits of detection (LODs, S/N = 3) of the method were determined from 11 and 87 ng/L. The developed method was demonstrated to be applicable for the rapid and sensitive determination of 16 PAHs in real environmental water samples.     

海洛因滥用者唾液中毒品代谢物的SPE-GC/MS-SIM分析

本文首先考查了不同类型不同厂家的固相萃取柱的萃取效果,采用提取效果较好的50 mg/mL的Clean-screen CSDAUL01混合型强阳离子固相萃取柱,对唾液中的吗啡、可待因、6-单乙酰吗啡等3种鸦片类毒品进行提取后,将提取液吹干;再经MBTFA衍生化后,进行GC/MS-SIM检测。以乙基吗啡为内标,3种毒品的线性相关系数均大于0.99,线性范围为10～1000 ng/mL,相对回收率分别为85%～110%、94%～107%和75%～92%;相对标准偏差小于10%。3种毒品的检测限分别为2 ng/mL、1 ng/mL和2 ng/mL。该方法灵敏度高、重现性好、操作简便,可用于鸦片类毒品滥用者及中毒者唾液中的毒品及其代谢物的检测。     

Optimized ultrasound‐assisted extraction procedure for the analysis of opium alkaloids in papaver plants by cyclodextrin‐modified capillary electrophoresis

This study investigated the use of ultrasound‐assisted extraction to improve the extraction efficiency of morphine, codeine and thebaine from the papaver plants. Extraction conditions such as type of solvent, temperature, duration, frequency and power level of ultrasonic were optimized and the influences of different parameters on resolution of alkaloids in CE were studied. The optimized condition for CE separation includes a sodium phosphate buffer (100 mM, pH 3.0) containing 5 mM α‐CD. The optimized extraction conditions for ultrasound‐assisted extraction was an extraction time of 1 h, an ultrasonic frequency of 60 kHz with water–methanol (80:20) at 40°C as the extraction solvent. The LOD for alkaloids was found to be 0.1 μg/mL at a signal‐to‐noise ratio of 3:1. The RSDs for peak areas were in the range of 1.4–4.4%. The amounts of opium alkaloids (mg/100 g dried sample) in four Iranian papaver plants were found to be in the range of 7.8–8.7 (morphine), 5.5–9.5 (codeine) and 1.4–10.4 (thebaine). It should be emphasized that no cleanup of the filtered extract was required; hence, direct determination after extraction drastically simplifies the analytical process.     

Preconcentration of trace uranium from seawater with solid phase extraction followed by differential pulse polarographic determination in chloroform eluate

In the present study, an effective method is presented for the separation and preconcentration of uranium (VI) by solid phase extraction (SPE). For this purpose, U(VI) oxinate is formed by the reaction of U(VI) with 8-hydroxyquinoline and adsorbed onto the octylsilane (C-8) SPE cartridge. The analyte is completely eluted with chloroform and determined by differential pulse polarography. The SPE conditions were optimized by evaluating the effective factors such as pH, oxine concentration, type and concentration of buffer and masking agent. By the proposed method a preconcentration factor more than 100 was achieved. The average recovery of uranium (VI) oxinate (0.1 mg l(-1)) was 99.8%. The relative standard deviation was 1.6% for seven replicate determinations of uranyl ion in the solution with a concentration 20 mug l(-1). Some concomitant ions such as Ca(+2), Mg(+2) and Fe(+3) which interfere in extraction or determination process of uranium were masked with EDTA in aqueous phase during the extraction process. The proposed method was successfully used for the determination of uranium in Caspian Sea and Persian Gulf water samples.     

固相萃取膜技术用于自来水中丙烯酰胺的测定

开发了一种简便快速的固相萃取膜(SPE disk)技术,实现了对500 mL自来水中微量丙烯酰胺的富集,采用高效液相色谱法(HPLC)完成其定性和定量测定。比较不同填料的吸附情况,选择活性炭作为丙烯酰胺的最佳吸附剂。考察了洗脱剂种类、洗脱剂体积、洗脱速率和穿透体积等条件对萃取结果的影响,优化了色谱分离条件。经膜萃取过的丙烯酰胺在0.05～0.5 mg/L质量浓度范围内,其峰面积与质量浓度的线性关系良好,相关系数为0.998,检出限为20 ng/L。该方法对不同体积、不同浓度的丙烯酰胺溶液的回收率为94.12%～100.2%,相对标准偏差为2.09%～4.51%(n=3),自来水样品的加标回收率为79.96%。该方法操作简单、快速、灵敏度高,适合对水样中丙烯酰胺的测定。     

Purification of 3-indolylacetic acid by solid phase extraction

This paper deals with the use of solid-phase extraction (SPE) for the extraction and purification of 3-indolylacetic acid (IAA), the main and most important representative of the plant growth regulators auxins. The procedure is based on the use of C18-SPE columns in two steps. In the first one, raw extract in methanol:water (4:1) is applied on the column in order to remove neutral ballast. In the second step the eluate is diluted with water to a final methanol concentration of 20% (to decrease the elution strength of the solvent) and acidified with formic acid to a final concentration of 1% (to convert the IAA from the anionic to the neutral form). Neutral IAA is then retained on the second SPE column, eluted by (acidified) methanol, and subjected to final analysis. Scintillation counting of tritium labeled IAA standard was used for the investigation and optimization of the SPE procedure. Gas chromatography with mass spectrometric detection was suggested as a convenient method for routine determination of IAA after its methylation with diazomethane. Overall recovery of the procedure was estimated as 89-94% and a physiological level of IAA equal to 0.48 nmol/g (84 ng/g) fresh weight was found using an optimized SPE-GC-MS method.     

毛细管电泳叠加对比法测定阿片粉中吗啡的含量

 用毛细管区带电泳 ,以叠加对比法对阿片粉中的吗啡进行了定量分析 ,样品的回收率为 10 0 .6 % ,峰迁移时间的相对标准偏差 (RSD)不大于 2 .4 % ,相对迁移时间的RSD不大于 1.1% ,相对峰面积的RSD不大于 0 .5 1%。与内标对比工作曲线法作了比较 ,实验表明两种分析方法的结果无显著性差异 ,叠加对比法具有简便、快速、准确的优点 ,可用于样品中有效成分的快速定量。     

疏水整体柱在线固相萃取与高效液相色谱-串联质谱联用测定牛肝中5种阿维菌素类药物残留

建立了牛肝中5种阿维菌素类药物残留的疏水整体柱在线固相萃取结合高效液相色谱-串联质谱测定的方法。以疏水的聚(甲基丙烯酸丁酯-乙二醇二甲基丙烯酸酯)整体柱(10 mm×2.1 mm)作为固相萃取介质,考察了上样流动相和洗脱流速对阿维菌素类药物的萃取效果,优化了梯度洗脱流动相的种类及质谱条件。方法在1~100 μg/L范围内线性关系良好(r>0.995),定量限为5 μg/kg。在5、10、50、100 μg/kg添加水平的回收率为77.4%~98.4%,日内和日间相对标准偏差分别为4.46%~8.03%和4.79%~8.68%,并且该柱反复使用400次后未发现萃取效率降低。结果表明,该整体柱对牛肝中5种阿维菌素类药物能够有效萃取,并且可以重复使用。该方法简单,自动化程度高,可应用于常规阿维菌素类药物残留分析。     

固相萃取/气相色谱-质谱法测定玩具中10种有机物的迁移量

建立了玩具中10种有机物迁移量的固相萃取/气相色谱-质谱测定方法。样品在25 mL去离子水中迁移60min,得到的迁移液流经Chromabond Easy固相萃取柱,用乙酸乙酯洗脱5次,每次1 mL。洗脱液过滤膜后通过60m DB-624色谱柱分离,质谱进行检测,外标法定量。方法对于不同有机物的定量限(LOQ)在0.0...