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    Chinese Journal of Chromatography
    2017, Vol. 35, No. 12
    Online: 08 December 2017

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    Determination of fipronil and its metabolites in bird eggs by ultra-performance liquid chromatography-tandem mass spectrometry with dispersive solid phase extraction
    LI Jiong, ZHENG Xin, WANG Hongqing, QIU Hongyu
    2017, 35 (12):  1211-1215.  DOI: 10.3724/SP.J.1123.2017.08018
    Abstract ( 808 )   [Full Text(HTML)] () PDF (870KB) ( 285 )  

    An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed to determine fipronil and its metabolites (fipronil desulfinyl, fipronil sulfone and fipronil sulfide) in bird eggs. The samples were extracted with acetonitrile containing 0.1%(v/v) acetic acid, and then purified by a mixture of anhydrous sodium sulfate, octadecyl carbon silica gel (C18-N) sorbent and ethylenediamine-N-propyl carbon silica gel (NH2-PSA) sorbent. The analysis was performed by a UPLC-MS/MS system with Shim-pack GIST C18 column (50 mm×2.1 mm, 2 μm). The mobile phases consisted of methanol and 1 mmol/L ammonium acetate aqueous solution by gradient elution, and multiple reaction monitoring (MRM) mode with negative electrospray ionization was used. The effect of the dosages of anhydrous sodium sulfate, C18-N and NH2-PSA in cleaning-up agent was studied. The main influence factors and analytical conditions were modified. Four linear calibration curves were obtained with correlation coefficients r2 ≥ 0.9989. The recoveries were determined at three concentrations and ranged from 95.09%-103.26%. The limit of quantification (LOQ) was 0.2 μg/kg. It is suitable for the determination of fipronil and its metabolites in bird eggs.

    Rapid screening of fipronil and its metabolites in egg and egg products by solid phase extraction-liquid chromatography-quadrupole time-of-flight mass spectrometry
    GUO Dehua, SHI Yiyin, LI You, YI Xionghai, DENG Xiaojun, XIAO Wenqing, WANG Jian, LI Xiao, LIU Han, SHEN Weijian
    2017, 35 (12):  1216-1223.  DOI: 10.3724/SP.J.1123.2017.09026
    Abstract ( 632 )   [Full Text(HTML)] () PDF (1916KB) ( 212 )  

    A method for rapid screening of fipronil and its metabolites in egg and egg products was developed by liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (LC-QTOF MS). The samples were extracted by acid-acetonitrile, cleaned up by PRiME HLB SPE. The separation was performed on a Poroshell 120 EC C18 column (150 mm×3 mm, 2.7 μm) with gradient elution using water and acetonitrile as mobile phases. The target compounds were monitored under negative ionization mode with electrospray ionization (ESI) source and two databases of accurate mass and fragment ions were created. The matrix effects in four kinds of egg and egg products were considered and the quantification was carried out by internal standard method. The results demonstrated that the linear ranges were from 0.1 to 5 μg/L with good correlation coefficients (r2>0.99). The limits of detection (LODs, S/N>3) and limits of quantitation (LOQs, S/N>10) were 0.2 μg/kg and 1 μg/kg, respectively. The recoveries of fipronil and its metabolites in different matrixes spiked with 1, 2 and 5 μg/kg varied from 82.6%-98.1%, and the relative standard deviations (RSDs) were between 3.8%-9.9% (n=6). The method can effectively correct the ionization suppression. It is sensitive, accurate and suitable for the rapid screening of fipronil, fipronil sulfide, fipronil sulfone and fipronil desulfinyl in egg, egg noodle, cake and mayonnaise.

    Determination of fipronil and its metabolites in eggs and egg products with gas chromatography-negative chemical ionization-mass spectrometry
    SHEN Weijian, LIU Han, ZHANG Rui, YU Keyao, CAI Lisheng, LIU Yan, WANG Hong
    2017, 35 (12):  1224-1228.  DOI: 10.3724/SP.J.1123.2017.09033
    Abstract ( 914 )   [Full Text(HTML)] () PDF (847KB) ( 343 )  

    A method was established for the determination of fipronil and its metabolites in eggs and egg products with gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS). The targets were extracted from samples with acetonitrile, and followed by a simple cleanup step known as dispersive solid-phase extraction QuEChERS. The extracts were determined by GC-NCI-MS, and quantified by external standard method with matrix correction standard curves. The recoveries were in the range of 87.0% to 99.3% at four spiked levels (0.1, 2.0, 4.0 and 20.0 μg/kg), and all RSDs were not more than 12.7% for the four analytes. The linearity of the method was good between 0.005 and 0.10 mg/L, and all LOQs were less than 0.10 μg/kg. So this method can be used to determine the residues of fipronil and its metabolites in eggs and egg products

    Research progress of bonded chiral stationary phases
    CHEN Jiao, SHI Hao
    2017, 35 (12):  1229-1239.  DOI: 10.3724/SP.J.1123.2017.09017
    Abstract ( 613 )   [Full Text(HTML)] () PDF (2006KB) ( 398 )  

    Chiral separation is important in biological medicine and other fields. High performance liquid chromatography (HPLC) is widely used in chiral separation and analysis for its economic, rapid and efficient characteristics. Chiral stationary phase (CSP) is the key to achieve chiral resolution in HPLC. Meanwhile, the key to preparing effective CSP is the screening of chiral selector. In recent years, a lot of CSPs with different chiral selectors had been prepared. Silica gel immobilized CSP is especially attached great attention because of its high solvent tolerance and stability. In this paper, the new type of CSPs prepared by using chiral single molecules, polysaccharides, cyclodextrins, macrocyclic antibiotics, crown ethers, calixarenes and alkaloids as chiral selectors are summarized, and the development prospect of immobilized CSPs are also discussed.

    Preparation of organic-inorganic hybrid poly(ionic liquids) material and evaluation of the adsorption to dyes
    CHEN Yujie, XIE Mingxue, FENG Zhuo, DENG Qiliang
    2017, 35 (12):  1240-1244.  DOI: 10.3724/SP.J.1123.2017.08010
    Abstract ( 574 )   [Full Text(HTML)] () PDF (2602KB) ( 141 )  

    An organic-inorganic hybrid poly(ionic liquids) material was prepared by using allyl triethoxysilane and 1-vinyl-3-octyl imidazolium bromide ionic liquids via combining free radical polymerization with sol-gel process. The prepared hybrid poly(ionic liquids) material was characterized by infrared spectroscopy and scanning electron microscopy. The adsorption properties of the prepared material to common dyes such as tartrazine, sunset yellow, amaranth and allura red were investigated. The results showed that the prepared poly(ionic liquids) material had excellent adsorption properties to sunset yellow and allura red. The adsorption capacities were 29.20 and 86.17 mg/g, respectively. When the adsorption time was 5 min, the material showed a fast adsorption rate to allura red and sunset yellow, which were 87.5% and 72.8% of the balance adsorption capacities, respectively.

    Confirmation and analysis of the metabolites of pentachlorophenol in loaches using ultra-performance liquid chromatography-high resolution mass spectrometry
    PAN Shengdong, CHEN Xiaohong, HE Qian, LI Xiaohai, WANG Li, ZHOU Jian, JIN Micong
    2017, 35 (12):  1245-1250.  DOI: 10.3724/SP.J.1123.2017.09012
    Abstract ( 630 )   [Full Text(HTML)] () PDF (892KB) ( 180 )  

    A method for the characterization of the metabolite pentachlorophenol hydrogen sulfate (PCP-SO3H) of pentachlorophenol (PCP) in loaches was developed based on ultra-performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS). The loach samples exposed in low concentration of PCP solution were firstly crushed, then extracted by acetonitrile-water solution (70:30, v/v) containing 8% (v/v) triethylamine and purified by mixed anion exchange solid-phase extraction (SPE) cartridges. The chromatographic separation was carried out on a Waters ACQUITY BEH C18 column (100 mm×2.1 mm, 1.7 μm). The qualitative analysis of the metabolites of PCP was operated in a negative electrospray ion mode (ESI-) under full mass-data dependent MS2 (full mass-ddMS2) mode, and the data of quasi-molecular ion, isotope ions, and MS2 fragmentation ions of metabolites were obtained. The results revealed that the sulfonation was the main metabolic pathway for PCP in loaches, not the hydroxylation or glucuronate pathway. And the metabolite was found to be PCP-SO3H. Besides, with the increase of exposure time in PCP solution, the concentration of metabolite PCP-SO3H firstly increased; when the exposure time was up to 36 h, the concentration of metabolite in loach reached a maximum value; and then extending the exposure time, the concentration of PCP-SO3H gradually decreased. When the exposure time was up to 120 h, the concentration of PCP-SO3H in loaches reached a lowest value, and no significant change occurred for further time. The developed UPLC-HRMS method in this study could be used for the investigation of the metabolism of PCP in living beings.

    Determination of hydroxyproline in liver tissue by hydrophilic interaction chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry
    LIU Wei, QI Shenglan, XU Ying, XIAO Zhun, FU Yadong, CHEN Jiamei, YANG Tao, LIU Ping
    2017, 35 (12):  1251-1256.  DOI: 10.3724/SP.J.1123.2017.09020
    Abstract ( 406 )   [Full Text(HTML)] () PDF (889KB) ( 165 )  

    A method for the determination of hydroxyproline (Hyp) in liver tissue of mice by hydrophilic interaction chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry (HILIC-HRMS) was developed. The liver tissue samples of normal mice and liver fibrosis mice induced by carbon tetrachloride were hydrolyzed by concentrated hydrochloric acid. After filtrated and diluted by solution, the diluent was separated on an Hypersil GOLD HILIC column (100 mm×2.1 mm, 3 μm). Water-acetonitrile (28:72, v/v)were used as the mobile phases with isocratic elution. Finally, the target analytes were detected in positive model by HRMS equipped with an electrospray ionization source. The linear range of hydroxyproline was from 0.78 to 100.00 μg/L with the correlation coefficient (R2) of 0.9983. The limit of quantification was 0.78 μg/L. By detecting the spiked samples, the recoveries were in the range of 97.4%-100.9% with the relative standard deviations (RSDs) between 1.4% and 2.0%. In addition, comparison of the measurement results by this method and the chloramine T method was proceeded. It was found that the linear correlation between the two methods was very good, and the Pearson correlation coefficient was 0.927. And this method had simpler operation procedure and higher accuracy than chloramine T method. This method can be used for the quick determination of hydroxyproline in liver tissue samples.

    Determination of 21 illegally added chemical drugs in health foods using ultra performance liquid chromatography-tandem mass spectrometry coupled with QuEChERS
    ZHENG Jia, XI Cunxian, CAO Shurui, WANG Guomin, TANG Bobin, WANG Zhi, MU Zhaode
    2017, 35 (12):  1257-1265.  DOI: 10.3724/SP.J.1123.2017.09031
    Abstract ( 541 )   [Full Text(HTML)] () PDF (1910KB) ( 179 )  

    A method for the simultaneous determination of 21 illegally added chemical drugs in improving sleep and immunity health foods using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. Oral liquid and health wine samples were shaken with acetonitrile and acetonitrile-water-formic acid (60:39:1, v/v/v), respectively, then purified by QuEChERS method. The extracts were separated on an Acquity UPLCTM BEH C18 column (50 mm×2.1 mm, 1.7 μm) with gradient elution of acetonitrile and 2 mmol/L ammonium acetate solution containing 0.1% (v/v) formic acid as mobile phases. The electrospray ionization in positive ion mode was used for analysis in multiple reaction monitoring (MRM) mode. The results showed that the target drugs had a good linear relationship in the range of 1-100 μg/L with the correlation coefficients (R2) ≥ 0.992. The limits of detection (LODs) and limits of quantification (LOQs) were 0.07-3.41 μg/kg and 0.22-11.36 μg/kg, respectively. The average recoveries of the 21 chemical drugs in oral liquid and health wine were in the range of 61.4%-116.5% and 67.4%-98.4% with the relative standard deviations (RSDs) of 0.2%-13.4% and 0.2%-11.8%, respectively. The developed method is sensitive and reliable. It has been successfully used for the detection of illegally added chemical drugs in real samples.

    Determination of 64 veterinary drug residues in aquatic products by ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry
    LI Rong, YANG Luqi, ZHANG Pengyun, LUO Yangdan, ZHANG Pengjie, GAO Yongqing
    2017, 35 (12):  1266-1275.  DOI: 10.3724/SP.J.1123.2017.08021
    Abstract ( 527 )   [Full Text(HTML)] () PDF (7927KB) ( 98 )  

    A method has been developed for the simultaneous determination of 64 veterinary drugs in aquatic products using ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry. The samples were extracted with an acetonitrile/water mixture (80/20, v/v), cleaned up by normal hexane saturated with acetonitrile and primary secondary amine (PSA) adsorbent, quantified with external standard method. The drugs were analyzed in full scan/data dependent mass spectrum 2 (Full MS/ddMS2) Top 1 mode. The calibration curves of the 64 drugs were linear with the correlation coefficients more than 0. 9967. The average recoveries of the 64 analytes ranged from 56.2% to 124.6%, and the relative standard deviations (RSDs) were 1.3%-29.8% in the three kinds of matrixes (fish, shrimp and shell) at three levels. The limits of quantification were 0.2-10 μg/kg. The method is simple, rapid, sensitive, reliable and suitable for the screening of residues in aquatic products.

    Simultaneous determination of seven avermectin residues in aquatic products by modified QuEChERS combined with high-performance liquid chromatography-tandem mass spectrometry
    LIU Yongtao, YU Linxue, WANG Zhenyue, YANG Qiuhong, DONG Jing, YANG Yibin, AI Xiaohui
    2017, 35 (12):  1276-1285.  DOI: 10.3724/SP.J.1123.2017.09019
    Abstract ( 602 )   [Full Text(HTML)] () PDF (1905KB) ( 362 )  

    A method was established for the simultaneous determination of seven avermectin (AVMs) residues, such as avermectin, ivermectin, doramectin, selamectin, eprinomectin, moxidectin and emamectin, in aquatic products using modified QuEChERS and high-performance liquid chromatography -tandem mass spectrometry (HPLC-MS/MS). The samples were extracted with 0.2% (v/v) ammoniate acetonitrile, and then 3 g of anhydrous magnesium sulfate and 2 g of anhydrous sodium sulfate were added to remove moisture and precipitate proteins. The samples were purified with 100 mg of C18 and 500 mg of anhydrous magnesium sulfate. The mobile phases comprised of acetonitrile (containing 0.1% (v/v) formic acid and 5 mmol/L ammonium acetate) and water (containing 0.1% (v/v) formic acid and 5 mmol/L ammonium acetate). The prepared samples were separated on a Varian Pursuit ULTRA C8 column (100 mm×2.0 mm, 2.8 μm) and determined using heated electrospray ionization (HESI) in the positive ion multiple reaction monitoring (MRM) mode. The analytes were quantified using external standard with the matrix-matched standard calibration curve method. The results showed that the solvent and matrix-matched standard curves for avermectin, ivermectin, doramectin, selamectin, eprinomectin and moxidectin in the range of 2-200 μg/L and for emamectin in the range of 0.2-20 μg/L were all linear, and the correlation coefficients (r) were ≥ 0.9972. The recoveries were 71.6%-112.8% with the relative standard deviations in the range of 4.7%-13.1%. The limits of quantification (LOQs) for avermectin, ivermectin, doramectin, selamectin, eprinomectin and moxidectin were all 5 μg/kg and for emamectin was 0.25 μg/kg. The present method is simple, repeatable, and suitable for the simultaneous determination of the residues of the seven avermectins in aquatic products.

    Simultaneous rapid determination of 12 microcystins and one nodularin in water by direct injection-ultra performance liquid chromatography-triple quadrupole mass spectrometry
    ZHANG Xiuyao, CAI Xinxin, ZHANG Xiaoyi, LI Ruifen
    2017, 35 (12):  1286-1293.  DOI: 10.3724/SP.J.1123.2017.09002
    Abstract ( 492 )   [Full Text(HTML)] () PDF (1240KB) ( 149 )  

    A rapid method was developed for the simultaneous determination of 12 microcystins (MCs) and one nodularin (NOD) in water by direct injection-ultra performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS). The water samples were first diluted with equal volume of methanol, and then filtered through polyether sulfone (PES) syringe filter. The filtrates were directly injected into the UPLC system. The separation of the analytes was carried out on an ACQUITY UPLC BEH 300 C18 column (100 mm×2.1 mm, 1.7 μm) with gradient elution using mobile phases of acetonitrile containing 0.1% (v/v) formic acid and 0.2% (v/v) formic acid aqueous solution. The 12 microcystins and one nodularin were detected by positive electrospray ionization in the multiple reaction monitoring (MRM) mode, and quantified by standard solvent external standard method. The limits of detection were 0.03-0.1 μg/L and the limits of quantification were 0.1-0.3 μg/L. The recoveries were in the range of 79.5%-123% with the relative standard deviations ranging from 1.0% to 20% (n=6). The method is simple, sensitive and accurate, and has been successfully applied to the detection of the 13 kinds of algae toxins in water.

    Determination and identification of acrylamide residues in poly-acrylamide by ultra-performance liquid chromatography-quadrupole electrostatic field orbitrap high-resolution mass spectrometry
    WANG Chenglong, ZHAO Jinli, LI Yanying, LIANG Lanlan, QI Ping
    2017, 35 (12):  1294-1300.  DOI: 10.3724/SP.J.1123.2017.08014
    Abstract ( 461 )   [Full Text(HTML)] () PDF (1637KB) ( 145 )  

    A new method for the direct determination of acrylamide residues in poly-acrylamide (PAM) by ultra-performance liquid chromatography (UPLC)-quadrupole electrostatic field orbitrap high-resolution mass spectrometry with the Hypercarb column was developed. With being diluted by water, the PAM sample was dissolved well by high-speed stirring. After filtering through a 0.22 μm aqueous phase microporous membrane, the sample was analyzed by high-resolution mass spectrometry directly. Chromatographic analysis was carried out using a Hypercarb column, distilled water and methanol applied as the mobile phases. In addition, the column temperature was strictly set at 20℃. The sample was determined in the mode of parallel reaction monitoring (PRM). Accurate mass-to-charge ratio extraction of the target compound ion and its fragment ion were utilized with elemental composition analysis and isotope distribution of the fragment ion to further improve the accuracy of qualitative and quantitative analysis. Meanwhile, the fragmentation pattern of acrylamide was acquired. The calibration curve showed a good linearity in the range of 2-50 μg/L with the correlation coefficient of 0.9998. The limit of detection (LOD) was 1.5 μg/kg, satisfying the detection demands. The recoveries of the acrylamide were in the range of 101.3%-107.1%. The relative standard deviations (RSD) were 3.1%-4.1%. The applications indicated that the mass percentages of AM in PAM were in the range of 0-0.43%. The proposed method is easy, fast, sensitive and suitable for the determination and confirmation of acrylamide residues in PAM.

    Determination of total phthalates in perfume and their exposure assessment
    ZHAO Sihan, WANG Zhengmeng, DENG Hongxia, DUAN Jiahui, WANG Jinyi, LIU Shuhui
    2017, 35 (12):  1301-1305.  DOI: 10.3724/SP.J.1123.2017.08026
    Abstract ( 443 )   [Full Text(HTML)] () PDF (1163KB) ( 182 )  

    A novel method for rapid screening of phthalates (PAEs) in perfumes was developed. The PAEs were hydrolyzed to phthalic acid (PA), and the PA in the acidified solution was extracted with tributyl phosphate (TBP) which was detected by high performance liquid chromatography-diode array detection (HPLC-DAD). Meanwhile exposure dose to PAEs was estimated by the percentage of a topically applied dose that permeates the skin. The parameters such as the concentration and volume of KOH, the volume of ethanol, hydrolysis time and temperature were employed to evaluate the hydrolysis efficiency of PAEs. The optimized hydrolysis conditions were 10 mL of 4 mol/L KOH, and 1 mL of ethanol at 80℃ for 20 min. The linear range of phthalic acid was 3-240 μmol/L with a good correlation coefficient (R2=0.9991). The limits of detection (LOD) and quantification (LOQ) were 4.6 μmol/kg and 5.9 μmol/kg, respectively. The recoveries varied from 83.4% to 92.7% with relative standard deviations equal to or lower than 6.8%(n=5). A total of 35 perfume samples were determined, and the contents of total PAEs were found in the range of

    Simultaneous determination of three benzimidazole fungicides in fruits and vegetables by capillary electrophoresis based on bacterial cellulose
    LIU Cuicui, BI Xiaotong, ZHANG Ailin, YAN Shijie
    2017, 35 (12):  1306-1311.  DOI: 10.3724/SP.J.1123.2017.09016
    Abstract ( 434 )   [Full Text(HTML)] () PDF (879KB) ( 96 )  

    A simple and rapid capillary electrophoresis (CE) method was developed for the determination of trace thiophanate-methyl, carbendazim and benomyl in fruits and vegetables. Herein, bacterial cellulose (BC) was used as additive in running buffer to improve the separation efficiency. CE experimental parameters such as detection wavelength, concentration and pH of the running buffer, separation voltage as well as the contents of BC in running buffer were systematically investigated. Under the optimized conditions, three benzimidazole fungicides could be accurate quantified in 8 min using H3BO3/Na2B4O7 (4 mmol/L, pH 9.0) containing 0.3% (mass fraction) BC for background electrolyte, 15 kV for the separation voltage, 25℃ for the column temperature and 275 nm for detection wavelength. Good linearities for the three benzimidazole fungicides were obtained with correlation coefficients (r2) ≥ 0.997. The limits of detection (LODs) of the three benzimidazole fungicides were between 5.0 and 10.0 μg/L. The relative standard deviations (RSDs, n=5) of inter-day were 0.82%-1.0% for retention times and 2.4%-2.9% for peak areas. The proposed method was further applied to determine the residues of the three benzimidazole fungicides in fruits and vegetables. The recoveries were in the range of 93.5%-103.0% with RSDs no more than 8.0%. These results indicated that the proposed method can serve as an efficient tool for the simultaneous determination of the three benzimidazole fungicides in fruits and vegetables.

    Analysis on metabolites with small molecule of serum in bone marrow suppression model mice with metabolomics method
    CHEN Jing, LIU Yunxia, XU Yefeng, WANG Yiqing
    2017, 35 (12):  1312-1316.  DOI: 10.3724/SP.J.1123.2017.08003
    Abstract ( 621 )   [Full Text(HTML)] () PDF (856KB) ( 251 )  

    Bone marrow suppression is a common symptom in patients with malignant tumor after chemotherapy. Studying the changes of metabolites caused by bone marrow depression can provide insights for the diagnosis of bone marrow suppression disease and for the development of drug therapy. Male BalB/C mice were injected with cyclophosphamide to establish a bone marrow suppression model. Gas chromatography-mass spectrometry (GC-MS) with fingerprinting was used to analyze the normal and model mice blood metabolites. Principal component analysis and orthogonal to partial least squares discriminant analysis (OPLS-DA) on metabolomics for data multidimensional statistical analysis was also used. Compared to the normal group in terms of the metabolic profile of bone marrow suppression mice, there were 15 endogenous metabolites in mouse plasma, nine of which were statistically significantly different, including glucose-1-phosphate, 4-nitrophenol, acetanilide, cortisone, nicotinamide, loganin, caffeic acid, linoleic acid and oleic acid (P<0.05). These results indicate that metabolite can be used as an important marker in bone marrow suppression, which can help to reveal the pathogenesis of bone marrow suppression induced by chemotherapy and determine the disease development stage and the effectiveness of follow-up treatment.

    Determination of six amide herbicide residues in soil by QuEChERS-gas chromatography-mass spectrometry
    MEI Wenquan, LI Qiwan, FANG Haixian, GENG Huichun, CHEN Xinglian
    2017, 35 (12):  1317-1321.  DOI: 10.3724/SP.J.1123.2017.09003
    Abstract ( 648 )   [Full Text(HTML)] () PDF (868KB) ( 156 )  

    A method was developed for the determination of six amide herbicides, such as acetochlor, alachlor, metolachlor, metazachlor, butachlor and pretilachlor, by QuEChERS-gas chromatography-mass spectrometry. The soil samples were extracted by 10 mL acetonitrile, 10 mL deionized water and 4 g sodium chloride, then purified with 50 mg N-propyl ethylenediamine (PSA), 50 mg C18, 10 mg graphitized carbon black (GCB) and 100 mg MgSO4. Low-polar silica capillary column HP-5MS was used. The extracts were detected by electron impact ionization (EI) source in the selected ion monitoring (SIM) mode. The results showed that good linearities were obtained with the mass concentrations of the six amide herbicides in the range of 0.01-1.00 mg/L, and their correlation coefficients ranged from 0.9996 to 1.0000. Under the condition of adding contents of 0.025, 0.10 and 0.50 mg/kg, the average recoveries of the six amide herbicides ranged from 92.0% to 108%, and the relative standard deviations were 1.64%-8.25%. The limits of detection (LODs) were 0.002-0.006 mg/kg and the limits of quantification (LOQs) were 0.005-0.02 mg/kg. Comparing with the gas chromatography-electron capture detection (GC-ECD) which used to detect the amide herbicides, this method can improve the anti-interference ability, and get better separation of the six amide herbicides. The method has the advantages of simplicity, rapidity, and application value.