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1.
王岚  方瑞斌  李忠  蒋次清  杨光宇 《色谱》2001,19(6):564-566
 建立了先用体积分数为 80 %的甲醇水溶液回流提取烟草样品中的植物多酚 ,再采用Sep Pak C18固相微萃取小柱预分离脱脂的前处理方法 ,并选择了合适的分析烟草样品中植物多酚的高效液相色谱条件。采用C18柱 ,甲醇 磷酸二氢钾缓冲液为流动相进行梯度洗脱 ,烟草中主要的植物多酚均达到基线分离。提取各组分在其最大波长下的色谱图 ,根据其峰面积定量 ,并用紫外光谱图对烟草中主要的植物多酚进行辅助定性。在该方法中 ,多酚的标准回收率为 94%~ 10 5 %,RSD为 1 2 8%~ 1 49%。该方法可用于烟草样品中的植物多酚的测定。  相似文献   

2.
固相萃取-气相色谱法测定水中毒死蜱   总被引:1,自引:0,他引:1  
水样中的毒死蜱经全自动固相萃取仪萃取、乙酸乙酯洗脱后,用气相色谱火焰光度检测法测定,以保留时间定性,外标法定量.结果表明:选用ENVI-18小柱萃取、乙酸乙酯洗脱,在2mL/min的过水速率下取得了良好的回收率.方法的线性范围为0.25~4.0mg/L.r为0.9998,回收率为88.6%~100.6%,相对标准偏差为2.58%~7.34%,最低定量浓度为2.5μg/L.本方法快速、灵敏、准确,并能够很好的排除干扰,可以满足水中痕量毒死蜱的测定.  相似文献   

3.
建立了固相萃取-表面增强拉曼光谱法(SPE-SERS)测定奶粉中三聚氰胺的分析方法。待测物经乙腈提取、活性碳吸附及氢氧化钠溶液洗脱后进行SERS检测。该方法的线性范围为0.0050~1.6mg/L,检出限为0.100mg/kg,回收率为75.3%~125%,相对标准偏差(RSD,n=5)不大于9.3%。该法灵敏度高、杂质干扰小、结果准确可靠,能满足奶粉中三聚氰胺的快速检测,在奶粉质量监控方面具有良好的应用潜力。  相似文献   

4.
固相萃取-液相色谱-串联质谱法检测食品中的三聚氰胺   总被引:14,自引:2,他引:14  
样品经均质,1%三氯乙酸溶液提取,用OASIS MCX固相萃取小柱净化,减压浓缩后以甲醇溶解定容,用Waters BEH-C8柱分离,乙腈和水为流动相,经液相色谱-串联质谱法检测.三聚氰胺线性范围为0.1~10.0mg/kg,相关系数r为0.9999,平均回收率为71%~95%,相对标准偏差为4.56%~9.82%(n=6),方法的栓出限为0.5 mg/kg.  相似文献   

5.
固相萃取-液相色谱法测定方便面中苯并芘   总被引:1,自引:0,他引:1  
摘要:建立固相萃取、高效液相色谱测定方便面中苯并芘的方法。采用正己烷作为萃取溶剂,经苯并芘检测专用固相萃取柱ProElut BaP净化提取,用高效液相色谱仪对方便面中苯并芘的含量进行测定。在0.5~10.0 μg/kg范围内苯并芘的质量浓度与色谱峰面积呈良好的线性关系,相关系数为0.9992,方法的检出限为0.3 μg/kg。调味包和面饼中苯并芘的加标回收率分别为86.3%~95.7%和88.8%~96.6%,测定结果的相对标准偏差分别为3.2%~3.5%和2.7%~3.2%(n=6)。该方法适合方便面中苯并芘含量的日常检测。  相似文献   

6.
提出了高效液相色谱法测定汤料中罂粟壳提取物吗啡、可待因和罂粟碱残留量的方法。样品用乙醚萃取,经离心分离,取上清液通过固相萃取柱纯化。流出液经过滤后,取10μL进样,在Zorbax SB C18色谱柱上进行分离,以不同比例混合的乙酸铵溶液和甲醇作为流动相进行梯度淋洗。吗啡、可待因和罂粟碱的线性范围均为0.05~50mg....  相似文献   

7.
建立了固相萃取-高效液相色谱法测定水产品中喹乙醇的方法。匀浆后的水产品试样经甲醇溶液提取、正己烷除脂、固相萃取小柱直接净化浓缩后,以体积分数15%的甲醇溶液作为流动相,流速:1.0 m L/min,采用Symmetryshield TM RP18色谱柱进行分离,紫外检测器检测,外标法定量。方法的检出限和定量限分别为0.02 mg/kg和0.05 mg/kg,浓度在0.05~1.00 mg/L范围内,线性良好(r=0.9999)。添加浓度在0.05~1.00 mg/kg时,不同品种水产品的回收率在78%~99.6%之间,相对标准偏差小于7.7%。方法适合于水产品样品的成批定量检测。  相似文献   

8.
以三聚氰胺为模板分子制备了三聚氰胺分子印迹聚合物(MIP),并将此聚合物装入自制的漏斗型固相萃取柱(SPE),制成对三聚氰胺有特异分子识别能力的SPE小柱。称取样品溶液10mL,以0.5mL·min-1速率流经SPE小柱,依次用水和甲醇-水(1+1)混合液各5mL淋洗小柱后,用甲醇-氨水(95+5)混合液8mL自然洗脱,将洗脱液吹氮蒸干,用甲醇1mL溶解残渣,所得溶液用于高效液相色谱分析。选用Inertsil ODS-SP C18色谱柱及(A)pH 3.0的10mmol·L-1辛烷磺酸钠-10mmol·L-1柠檬酸混合溶液和(B)乙腈以90比10比例相混的混合液作为流动相进行色谱分离。检测波长为240nm。在3个浓度水平进行回收试验,测得回收率在89.0%~97.0%之间。  相似文献   

9.
何强  孔祥虹  赵洁  李建华  乐爱山  张莹 《色谱》2008,26(5):563-567
建立固相萃取-离子交换色谱法测定浓缩苹果汁中苯菌灵、多菌灵和噻菌灵的残留量。样品直接用水稀释后,于80 ℃下将苯菌灵完全转化为多菌灵,再经SCX固相萃取柱富集,采用LC-SCX离子交换色谱柱(25 cm×4.6 mm,5 μm)分离,二极管阵列检测器检测,以0.1 mol/L KH2PO4溶液(pH 2.5)-乙腈(体积比为70 ∶30)为流动相,在1.0 mL/min下等度洗脱,于282 nm波长下检测。在0.02~2.0 mg/L范围内,多菌灵和噻菌灵的峰面积与其浓度呈良好的线性关系,最低检出限均可达到0.004 mg/kg,回收率为94.2%~100.4%,相对标准偏差低于4.2%。该方法简便、快速、灵敏、准确,可用于浓缩苹果汁中苯菌灵、多菌灵和噻菌灵残留量的检测。  相似文献   

10.
建立了固相萃取-亲水相互作用色谱/串联质谱同时测定食品中三聚氰胺和三聚氰酸残留量的方法。采用乙腈和水提取试样中残留的三聚氰胺和三聚氰酸,正己烷脱脂,提取液经亲水性键合硅胶和阳离子交换树脂复合填料柱(MCT柱)净化。采用亲水相互作用色谱柱进行分离,质谱采用正、负离子切换模式电离,多反应监测模式检测,同位素内标法定量。三聚氰胺和三聚氰酸在10~2500 μg/L范围内呈线性相关,相关系数(r)均大于0.99,定量限分别为25和50 μg/kg。本方法在动物源性食品、植物源性食品、乳及乳制品等不同样品中的三聚氰胺和三聚氰酸高、中、低3个添加水平的回收率分别在70.0%~129.6%和70.0%~128.6%之间,相对标准偏差分别在1.4%~23.3%和2.8%~18.7%之间。该方法可满足食品中三聚氰胺和三聚氰酸同时定量测定的需要。  相似文献   

11.
12.
优化建立了采用混合模式阳离子交换固相萃取柱代替传统的C18固相萃取柱进行前处理,联用高效液相色谱检测河豚鱼中河豚毒素的方法.样品经合1%乙酸的乙腈甲醇(3:1,V:V)溶液提取,混合模式阳离子交换固相萃取柱(MCX)净化,5%氨水/甲醇溶液洗脱,采用高效液相色谱-二极管阵列检测器(HPLC-PAD)测定,外标法定量.河...  相似文献   

13.
Summary An analytical method has been developed to determine the chloroethene series, tetrachloroethene (PCE), trichloroethene (TCE),cisdichloroethene (cis-DCE) andtransdichloroethene (trans-DCE) in environmental biotreatment studies using gas chromatography coupled with a solid phase micro extraction (SPME) technique. The volatile chlorinated compounds in aqueous solution can be analyzed directly without solvent extraction, purge and trap, or thermal heating. The calibration curves have demonstrated good linear relationships within 50.0 to 3000.0 g L–1 concentration range. Detection limits are 18.0, 5.0, 25.0, and 42.0 g L–1, for PCE, TCE,cis-DCE andtrans-DCE, respectively. Factors which affect the SPME process, such as sample adsorption time, thermal desorption time, and concentration of salt in the matrix, have also been evaluated.  相似文献   

14.
A new method for determination of volatile terpenoids in wine is proposed. An off-line solid phase extraction—gas chromatographic method has been used for the determination. The influence of several extraction variables was studied, including the solid phase employed (C-18 versus divinylbenzene-based), eluting solvent (n-pentane, dichloromethane, ethanol and methanol), volume of eluting solvent (1-4 ml) and drying time (0-20 min). Complete recovery of volatile terpenoids from several kinds of wines was obtained under the optimized conditions.  相似文献   

15.
A new method is described for the determination of famotidine by solid phase extraction from alkalinized human plasma followed by reversed phase (RP) HPLC in acetonitrile/alkaline buffer with molsidomine as an internal standard. Different acetonitrile/aqueous buffer mobile phases as well as various RP columns were used. Alkaline medium allowed the limit of quantitation to be lowered to 5 ng/mL of plasma as the famotidine gives more intense absorption at about 286 nm (at pH values higher than 7). Moreover, work in alkaline media and at this wavelength is highly selective as peaks corresponding to impurities present in most samples are well separated. A method using a mildly alkaline mobile phase (acetonitrile/10 mM phosphate with 10 mM 1‐heptanesulphonic acid, pH 7.5) was successfully used for determination of famotidine in human plasma in a pharmacokinetic study.  相似文献   

16.
采用固相萃取(SPE)前处理净化技术,高效液相色谱(HPLC)测定动物组织中盐酸莱克多巴胺残留量,通过对样品中待测组分的提取、净化,建立了反相高效液相色谱(RP-HPLC)测定动物组织中盐酸莱克多巴胺残留量。线性范围为1.0~100μg/L;相关系数大于0.9998;检出限0.3μg/L;3个不同水平标准添加回收率(n=7)为89.3%~100.5%;相对标准偏差(RSD)为3.9%~5.0%。  相似文献   

17.
This paper presents a novel analytical method for the determination of pyridinium ionic liquid cations in environmental water samples by ion chromatography coupled with solid phase extraction. The water samples were purified and enriched by a sulphonic acid extraction column, and then the impurities were washed with 10 mL water – 20% (v/v) acetonitrile solution and the analytes eluted with 0.5 mol L?1 phosphoric acid – sodium dihydrogen phosphate buffer solution – 55% methanol. The eluted analytes were determined by ion chromatography with 3.0 mmol L?1 methane sulphonic acid – 8% acetonitrile as the mobile phase and direct conductivity detection. Three pyridinium cations were completely separated in 20 min and the retention mechanism basically conforms to the ion exchange mode. The newly developed method has been successfully applied to the analysis of pyridinium cations in spiked environmental water samples, which provided satisfactory recoveries in the range of 98.8% to 100.0% with the relative standard deviations less than 2.8%. The concentration of 0.004 to 0.01 mg L?1 in water samples can be preconcentrated by this method. The method is accurate, reliable, simple and practical. This research provides a new reference for detecting ionic liquid cations in environmental water samples and studying the environmental risk assessment of ionic liquids.  相似文献   

18.
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).  相似文献   

19.
Summary Flavanones ofArachis hypogaea, Hemizonia increscens, Eriodictyon glutinosum andThymus vulgaris extracts have been stereospecifically analysed by gradient elution on a column of cellulose triacetate supported on silica gel diol. The stereochemistry of naringenin, eriodictyol and homoeriodictyol was in favour of the 2S-configurated flavanones.  相似文献   

20.
建立了利用淋洗液自动发生梯度淋洗的离子交换色谱法同时测定水产品中酪胺、5-羟色胺、腐胺、尸胺、组胺、庚二胺、苯乙胺、亚精胺、精胺、色胺等10种生物胺的方法.样品经处理后用Ionpac CS17分离柱和Ionpac CG17型保护柱分离,以EG40自动淋洗液发生器生成的5.0~55 mmol/L的MSA为淋洗液梯度洗脱,脉冲积分安培检测器检测.对梯度进行优化,10种生物胺都能基线分离,并且浓度和峰面积在一定范围内呈良好的线性关系.检出限在0.04 mg/kg以下,回收率在91.2%~102.5%之间,样品的RSD(n =6)小于5%.方法可用于水产品的检测.  相似文献   

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