QuEChERS-超高效液相色谱法检测瓜果中14种植物生长调节剂残留量
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摘要
目的建立QuEChERS-超高效液相色谱法同时检测黄瓜、番茄等瓜果中14种植物生长调节剂残留量。方法样品经含0.5%甲酸的乙腈-二氯甲烷(1∶1,V/V)提取、分散固相萃取法净化,采用Agilent InfinityLab Poroshell 120 EC-C_(18)色谱柱(4.6 mm×100 mm, 2.7μm),0.05%乙酸和乙腈为流动相梯度洗脱,在220、254 nm同时进行检测。结果 14种植物生长调节剂在12 min内实现快速分离,在线性范围内的相关系数(r)均大于0.999,检出限为0.005～0.076 mg/kg,定量限为0.02～0.32 mg/kg,加标回收率为71.9%～113.8%,相对标准偏差(RSD)均小于5.0%。结论该方法能同时快速检测多种植物生长调节剂。操作简单,具有较好的灵敏度、精密度及回收率,检测成本低,适用于大批量样品的定量筛查。
Objective A method for the simultaneous determination of 14 plant growth regulator residues in cucumbers and tomatoes, etc. by QuEChERS-ultra-high performance liquid chromatography(UPLC) was developed. Methods The samples were extracted by CH_2Cl_2-CH_3CN(1∶1,V/V) containing 0.5% formic acid, and purified with dispersive solid phase extraction. Chromatographic analysis was carried out on Agilent InfinityLab Poroshell 120 EC-C_(18) column(4.6 mm×100 mm, 2.7 μm) with acetonitrile-0.05% acetic acid as the mobile phase using gradient elution, and detected at 220 and 254 nm. Results Rapid separation of 14 analytes could be performed in 12 minutes. The correlation coefficients of calibration curves were above 0.999. The limits of detection and quantification were in the ranges of 0.005-0.076 mg/kg and 0.02-0.32 mg/kg. The average recoveries varied from 71.9% to 113.8% with relative standard deviations less than 5.0%. Conclusion The method was rapid for simultaneous determination of varied residues. It was simple,reliable and cost-effective and was suitable for quantitative screening of large quantities of samples.
Objective A method for the simultaneous determination of 14 plant growth regulator residues in cucumbers and tomatoes, etc. by QuEChERS-ultra-high performance liquid chromatography(UPLC) was developed. Methods The samples were extracted by CH_2Cl_2-CH_3CN(1∶1,V/V) containing 0.5% formic acid, and purified with dispersive solid phase extraction. Chromatographic analysis was carried out on Agilent InfinityLab Poroshell 120 EC-C_(18) column(4.6 mm×100 mm, 2.7 μm) with acetonitrile-0.05% acetic acid as the mobile phase using gradient elution, and detected at 220 and 254 nm. Results Rapid separation of 14 analytes could be performed in 12 minutes. The correlation coefficients of calibration curves were above 0.999. The limits of detection and quantification were in the ranges of 0.005-0.076 mg/kg and 0.02-0.32 mg/kg. The average recoveries varied from 71.9% to 113.8% with relative standard deviations less than 5.0%. Conclusion The method was rapid for simultaneous determination of varied residues. It was simple,reliable and cost-effective and was suitable for quantitative screening of large quantities of samples.
引文
[1] 苏杭, 张鹏, 李慧, 等. 我国常用植物生长调节剂对水果品质影响研究[J]. 农产品质量与安全,2017(2):44-48.
[2] 陈卫军, 张耀海, 李云成,等. 果蔬中常用植物生长调节剂分析方法研究进展[J]. 食品科学, 2012, 33(11):283-289.
[3] 苏明明,杨春光,李一尘,等. 植物生长调节剂对粮食作物、瓜果的影响及其残毒研究综述[J]. 食品安全质量检测学报,2014,5(8):2575-2579.
[4] 中华人民共和国国家卫生和计划生育委员会, 中华人民共和国农业部, 国家食品药品监督管理总局.食品安全国家标准食品中农药最大残留限量:GB 2763—2016 [S].北京:中国标准出版社,2016.
[5] JIANG X X, SHI H Y, WU N, et al. Development of an enzyme-linked immunosorbent assay for diniconazole in agricultural samples[J].Food Chemistry, 2011, 125(4): 1385-1389.
[6] 陈锡爱,武雪,张松,等. 基于太赫兹光谱的植物生长调节剂检测技术研究[J]. 光谱学与光谱分析, 2018, 38(3):665-669.
[7] AMER M M, SHEHATA M A, LOTFY H M, et al. Determination of tetraconazole and diniconazole fungicide residues in tomatoes and green beans by capillary gas chromatography[J]. Yakugaku Zasshi Journal of the Pharmaceutical Society of Japan, 2007, 127(6): 993-999.
[8] 张文华, 谢文, 侯建波,等. 气相色谱-串联质谱法测定豆芽与番茄中6种植物生长调节剂[J]. 分析测试学报, 2016, 35(10):1241-1247.
[9] 薛荣旋, 黄诚, 刘国平, 等. QuEChERS结合气相色谱-串联质谱法测定水果中5种植物生长调节剂[J]. 中国食品卫生杂志, 2017, 29(5):561-566.
[10] 朱松, 袁晓晴,戴军, 等. QuEChERS/HPLC/DAD法同时检测果蔬中多种植物激素残留[J].分析测试学报,2017,36(4):513-518.
[11] 邵金良,樊建麟,林涛,等. 高效液相色谱法同时测定果蔬中5种植物生长调节剂残留[J]. 食品安全质量检测学报, 2015, 6(8):3255-3261.
[12] 袁文新, 刘志平, 刘平, 等. 固相萃取-超高效液相色谱法同时测定豆芽中4种植物生长调节剂[J]. 卫生研究, 2017, 46 (5):783-787.
[13] 郝杰, 姜洁, 毛婷, 等. QuEChERS-超高效液相色谱-串联质谱法同时测定蔬果中34种植物生长调节剂的残留量[J]. 食品科学, 2018, 39(8):267-275.
[14] 邱暑婷, 林学飞, 傅冰梦, 等. QuEChERS/高效液相色谱-串联质谱法同时测定葡萄中18种植物生长调节剂残留[J]. 中国卫生检验杂志, 2017,27(7):931-936.
[15] 王炼, 骆春迎, 张礼春, 等. 液相色谱-串联质谱法测定水果中6种植物生长调节剂残留量[J]. 中国食品卫生杂志,2016,28(4):451-456.
[16] 周鸿艳, 黄方取, 刘洋, 等. QuEChERS高效液相色谱-串联质谱法测定多种水果中的6种植物生长调节剂的残留量[J]. 中国卫生检验杂志, 2016, 26(13):1847-1851.
[17] 黄何何,张缙,徐敦明,等. QuEChERS-高效液相色谱-串联质谱法同时测定水果中21种植物生长调节剂的残留量[J]. 色谱,2014, 32(7):707-716.
[18] 张泸文, 焦广睿, 王柯, 等. QuEChERS-高效液相色谱-串联质谱法同时测定果蔬中26种植物生长调节剂残留[J]. 食品安全质量检测学报, 2016,7(7):2677-2689.
[19] 金艳红,朱群英. QuEChERS耦合UPLC-MS/MS同时测定葡萄中9种植物生长调节剂[J]. 食品安全导刊,2017(21):144-149.
[20] 周纯洁, 赵博, 吴丹,等. QuEChERS-超高效液相色谱-串联质谱法同时测定蔬菜中6种植物生长调节剂[J]. 食品工业科技, 2016, 37(10):94-98.
[21] 牟艳莉, 郭德华, 丁卓平, 等. 高效液相色谱-串联质谱法测定瓜果中11种植物生长调节剂的残留量[J].分析化学,2013,41(11):1640-1646.
[22] WILKOWSKA A,BIZIUK M.Determination of pesticide residues in food matrices using the QuEChERS methodology[J]. Food Chem,2011,125(3):803-812.
[2] 陈卫军, 张耀海, 李云成,等. 果蔬中常用植物生长调节剂分析方法研究进展[J]. 食品科学, 2012, 33(11):283-289.
[3] 苏明明,杨春光,李一尘,等. 植物生长调节剂对粮食作物、瓜果的影响及其残毒研究综述[J]. 食品安全质量检测学报,2014,5(8):2575-2579.
[4] 中华人民共和国国家卫生和计划生育委员会, 中华人民共和国农业部, 国家食品药品监督管理总局.食品安全国家标准食品中农药最大残留限量:GB 2763—2016 [S].北京:中国标准出版社,2016.
[5] JIANG X X, SHI H Y, WU N, et al. Development of an enzyme-linked immunosorbent assay for diniconazole in agricultural samples[J].Food Chemistry, 2011, 125(4): 1385-1389.
[6] 陈锡爱,武雪,张松,等. 基于太赫兹光谱的植物生长调节剂检测技术研究[J]. 光谱学与光谱分析, 2018, 38(3):665-669.
[7] AMER M M, SHEHATA M A, LOTFY H M, et al. Determination of tetraconazole and diniconazole fungicide residues in tomatoes and green beans by capillary gas chromatography[J]. Yakugaku Zasshi Journal of the Pharmaceutical Society of Japan, 2007, 127(6): 993-999.
[8] 张文华, 谢文, 侯建波,等. 气相色谱-串联质谱法测定豆芽与番茄中6种植物生长调节剂[J]. 分析测试学报, 2016, 35(10):1241-1247.
[9] 薛荣旋, 黄诚, 刘国平, 等. QuEChERS结合气相色谱-串联质谱法测定水果中5种植物生长调节剂[J]. 中国食品卫生杂志, 2017, 29(5):561-566.
[10] 朱松, 袁晓晴,戴军, 等. QuEChERS/HPLC/DAD法同时检测果蔬中多种植物激素残留[J].分析测试学报,2017,36(4):513-518.
[11] 邵金良,樊建麟,林涛,等. 高效液相色谱法同时测定果蔬中5种植物生长调节剂残留[J]. 食品安全质量检测学报, 2015, 6(8):3255-3261.
[12] 袁文新, 刘志平, 刘平, 等. 固相萃取-超高效液相色谱法同时测定豆芽中4种植物生长调节剂[J]. 卫生研究, 2017, 46 (5):783-787.
[13] 郝杰, 姜洁, 毛婷, 等. QuEChERS-超高效液相色谱-串联质谱法同时测定蔬果中34种植物生长调节剂的残留量[J]. 食品科学, 2018, 39(8):267-275.
[14] 邱暑婷, 林学飞, 傅冰梦, 等. QuEChERS/高效液相色谱-串联质谱法同时测定葡萄中18种植物生长调节剂残留[J]. 中国卫生检验杂志, 2017,27(7):931-936.
[15] 王炼, 骆春迎, 张礼春, 等. 液相色谱-串联质谱法测定水果中6种植物生长调节剂残留量[J]. 中国食品卫生杂志,2016,28(4):451-456.
[16] 周鸿艳, 黄方取, 刘洋, 等. QuEChERS高效液相色谱-串联质谱法测定多种水果中的6种植物生长调节剂的残留量[J]. 中国卫生检验杂志, 2016, 26(13):1847-1851.
[17] 黄何何,张缙,徐敦明,等. QuEChERS-高效液相色谱-串联质谱法同时测定水果中21种植物生长调节剂的残留量[J]. 色谱,2014, 32(7):707-716.
[18] 张泸文, 焦广睿, 王柯, 等. QuEChERS-高效液相色谱-串联质谱法同时测定果蔬中26种植物生长调节剂残留[J]. 食品安全质量检测学报, 2016,7(7):2677-2689.
[19] 金艳红,朱群英. QuEChERS耦合UPLC-MS/MS同时测定葡萄中9种植物生长调节剂[J]. 食品安全导刊,2017(21):144-149.
[20] 周纯洁, 赵博, 吴丹,等. QuEChERS-超高效液相色谱-串联质谱法同时测定蔬菜中6种植物生长调节剂[J]. 食品工业科技, 2016, 37(10):94-98.
[21] 牟艳莉, 郭德华, 丁卓平, 等. 高效液相色谱-串联质谱法测定瓜果中11种植物生长调节剂的残留量[J].分析化学,2013,41(11):1640-1646.
[22] WILKOWSKA A,BIZIUK M.Determination of pesticide residues in food matrices using the QuEChERS methodology[J]. Food Chem,2011,125(3):803-812.