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低压顶空固相微萃取-气相色谱- 串联质谱法测定土壤中酞酸酯类化合物
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作者 何虹 《化学分析计量》 CAS 2020年第6期83-88,共6页
建立低压顶空固相微萃取-气相色谱-串联质谱法测定土壤中酞酸酯类化合物的分析方法。选取PDMS/DVB-65μm固相微萃取纤维,加入1 mL盐溶液,0.1kPa的顶空压力和80℃的萃取温度作为最佳实验条件,采用气相色谱-串联质谱法进行测定,外标法定量... 建立低压顶空固相微萃取-气相色谱-串联质谱法测定土壤中酞酸酯类化合物的分析方法。选取PDMS/DVB-65μm固相微萃取纤维,加入1 mL盐溶液,0.1kPa的顶空压力和80℃的萃取温度作为最佳实验条件,采用气相色谱-串联质谱法进行测定,外标法定量。6种酞酸酯类化合物的含量在5~800μg/kg范围内与色谱峰面积具有良好的线性关系,相关系数均不小于0.992,检出限为0.5~4.2μg/kg,定量限为1.7~14μg/kg。样品加标回收率为79.4%~102.8%,测定结果的相对标准偏差为7.5%~14.1%(n=5)。采用该方法和加速溶剂萃取法对实际土壤进行检测,结果表明,该方法对实际土壤中DMP,DEP,DBP,BBP,DEHP和DNOP 6种酞酸酯类化合物均具有较好的提取富集效果。该方法为土壤环境中酞酸酯类有机污染物的测定提供了更环保的技术手段。 展开更多
关键词 低压顶空 固相微萃取 酞酸酯类 气相色谱–串联质谱 土壤
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凝胶渗透色谱-气相色谱-串联质谱法测定牛奶中的两种光引发剂 被引量:8
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作者 陶运来 田素润 《化学分析计量》 CAS 2018年第5期11-15,共5页
建立了采用凝胶渗透色谱(GPC)为净化方式的牛奶中外源性光引发剂二苯甲酮(BP)和4-甲基二苯甲酮(MBP)的气相色谱–串联质谱(GC–MS/MS)测定方法。样品采用乙腈超声辅助提取,经环己烷–乙酸乙酯(体积比为1∶1)溶剂转化后用GPC净化,再通过H... 建立了采用凝胶渗透色谱(GPC)为净化方式的牛奶中外源性光引发剂二苯甲酮(BP)和4-甲基二苯甲酮(MBP)的气相色谱–串联质谱(GC–MS/MS)测定方法。样品采用乙腈超声辅助提取,经环己烷–乙酸乙酯(体积比为1∶1)溶剂转化后用GPC净化,再通过HP–5MS气相色谱柱分离,最后经串联四极杆质谱仪检测器进行定性、定量同时分析。该方法的线性范围为5~100μg/L,BP和MBP的线性相关系数(r2)分别为0.997 2和0.998 4,方法定量限均为0.025 mg/kg。在空白牛奶样品中加入0.05,0.25,0.50 mg/kg 3个浓度水平的BP和MBP,BP和MBP的平均回收率为74.0%~92.0%,测定结果的相对标准偏差为5.5%~10.9%(n=6)。该方法具有灵敏度高、准确度和精密度好的优点,适合牛奶中BP和MBP两种光引发剂的检测。 展开更多
关键词 凝胶渗透色谱 气相色谱–串联质谱 牛奶 光引发剂
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Determination of 10 Pyrethroids Pesticide Residues in Rice by GC-MS-MS 被引量:1
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作者 吴俐 曹赵云 +2 位作者 牟仁祥 林晓燕 陈铭学 《Agricultural Science & Technology》 CAS 2017年第8期1526-1530,共5页
[Objective] A method was developed for the determination of 10 pyrethroids pesticide residues in rice by GC-MS-MS. [Method] Pyrethroids were extracted with acetonitrile, followed by a salting-out step with anhydrous m... [Objective] A method was developed for the determination of 10 pyrethroids pesticide residues in rice by GC-MS-MS. [Method] Pyrethroids were extracted with acetonitrile, followed by a salting-out step with anhydrous magnesium sulfate and sodium chloride, cleaned up by florisil solid phase extraction (SPE) cartridge, and determined by multiple reaction monitoring mode. [Result] The method showed good linearity over the range of 0.010-0.500 mg/L for 10 pyrethroid pesticide with correlation coefficients over 0.99. The detection limits were 0.005 -0.010 mg/kg. The method was validated by analyzing samples spiked with 0.05, 0.10, 0.20 mg/kg of 10 pyrethroid pesticides, respectively. The average recoveries in rice ranged from 75.0-115.5%, and the relative standard deviations (RSD) were between 3.9%-6.9%. [Conclusion] The method is easy, accurate and reliable, which can meet the requirement for the simultaneous determination and confirmation of pyrethroid pesticide residues in rice. 展开更多
关键词 GC-MS-MS Pesticide residues RICE PYRETHROIDS PESTICIDE
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SPME-GC/MS测定异味食盐中脂肪酸组成
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作者 董榕贵 杨树江 于以竹 《药物化学》 2022年第3期287-291,共5页
建立一种SPME结合GC/MS测定异味食盐中脂肪酸组成的方法,样品用0.2%磷酸酸化,固相微萃取纤维头萃取,VF-WaxMS色谱柱分离,全扫描(Scan)方式扫描,经过NIST2.2谱库定性,面积归一化法定量。在异味食盐中共检出27种脂肪酸,其中12种脂肪酸为... 建立一种SPME结合GC/MS测定异味食盐中脂肪酸组成的方法,样品用0.2%磷酸酸化,固相微萃取纤维头萃取,VF-WaxMS色谱柱分离,全扫描(Scan)方式扫描,经过NIST2.2谱库定性,面积归一化法定量。在异味食盐中共检出27种脂肪酸,其中12种脂肪酸为短链脂肪酸,含量最高为异戊酸,达49.64%,15种脂肪酸为中长链脂肪酸,含量较低均在5%以下,结果表明,该方法操作简便,灵敏度高,适用于异味食盐的快速鉴别及其脂肪酸成分的测定。 展开更多
关键词 异味食盐 气相色谱–串联质谱 固相微萃取 脂肪酸
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Analysis and Evaluation of the Acrylamide Levels in Some Bread Assortments on the Romanian Market by GC-MS/MS
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作者 Mioara Negoita Enuta Iorga +5 位作者 Alina Adascalului Luminita Catana Nastasia Belc Andreea Stan DragosEfstatiade Hassan Y. Aboul-Enein 《Journal of Environmental Science and Engineering(A)》 2016年第4期180-189,共10页
The acrylamide level of some commercial bread assortments have been evaluated. The influence of several flour types on the content of acrylamide in 14 samples of bread, purchased from 5 different suppliers from the ma... The acrylamide level of some commercial bread assortments have been evaluated. The influence of several flour types on the content of acrylamide in 14 samples of bread, purchased from 5 different suppliers from the market in Bucharest, Romania was studied. For all bread assortments which have been analyzed for acrylamide, the International Commission of Illumination (CIELab) parameters, L*, a* and b* have been also measured in an attempt to correlate the colour of the final product with its acrylamide content. Determination of acrylamide in bread samples was performed by Gas Chromatography coupled with tandem Mass Spectrometry (GC-MS/MS), using isotope dillution calibration after derivatization (bromination). The results revealed that the acrylamide level vary between bread assortments of different brands and bread assortments of same brand, but different lots. In the case of commercial bread samples, the use of whole wheat flours lead to formation of higher quantity in acrylamide (165.53 μg/kg), compared to the use of white wheat flours (28.02μg/kg). 展开更多
关键词 ACRYLAMIDE FLOUR BREAD GC/MS/MS CIELab parameters.
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