改进的QuEChERS-超高效液相色谱-串联质谱法测定毛木耳中23种植物生长调节剂的残留量
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摘要
目的建立改进的QuEChERS-超高效液相色谱-串联质谱法测定毛木耳中23种植物生长调节剂的分析方法。方法样品经1%乙酸乙腈溶液提取后,比较了C_(18)和PEP-2的净化和去除色素能力,同时对提取试剂和PEP-2净化剂用量进行了优化,采用超高效液相色谱-串联质谱测定。结果在优化的条件下,23种植物生长调节剂在相关范围内线性关系良好(r>0.999),方法定量限为0.1～5μg/kg,在0.01、0.05、0.1 mg/kg 3个添加浓度下平行6次实验,回收率为80.6%～116.6%,RSD为0.9%～11.2%。结论该法满足国内外植物生长调节剂残留限量要求,可为食用菌中植物生长调节剂残留检测提供参考。
Objective To establish a method for determination of 23 plant growth regulators in Auricularia cornea by modified QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry(UPLS-MS/MS). Methods The samples were extracted with 0.1% acetic acetonitrile solution, then the capacity of purification and pigment removal of C_(18)and PEP-2 were compared. At the same time, the amount of extraction reagent and PEP-2 purifier was optimized, and samples were detected by UPLC-MS/MS. Results Under the optimum conditions, 23 plant growth regulators had linear relationships(r>0.999), and the limits of quantitation were ranged from 0.1 to 5 μg/kg. The recoveries at 3 spiked levels(0.01, 0.05 and O.lmg/kg) were 82.6%-116.6%, with the relative standard deviations(RSD) of 0.9%-11.2%(n=6). Conclusion This method is satisfied the demand of the plant growth regulators residue limits, which can provide technical support for detection of plant growth regulator residues in edible fungi.
Objective To establish a method for determination of 23 plant growth regulators in Auricularia cornea by modified QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry(UPLS-MS/MS). Methods The samples were extracted with 0.1% acetic acetonitrile solution, then the capacity of purification and pigment removal of C_(18)and PEP-2 were compared. At the same time, the amount of extraction reagent and PEP-2 purifier was optimized, and samples were detected by UPLC-MS/MS. Results Under the optimum conditions, 23 plant growth regulators had linear relationships(r>0.999), and the limits of quantitation were ranged from 0.1 to 5 μg/kg. The recoveries at 3 spiked levels(0.01, 0.05 and O.lmg/kg) were 82.6%-116.6%, with the relative standard deviations(RSD) of 0.9%-11.2%(n=6). Conclusion This method is satisfied the demand of the plant growth regulators residue limits, which can provide technical support for detection of plant growth regulator residues in edible fungi.
引文
[1]谭伟,苗人云,周洁,等.毛木耳栽培技术研究进展[J].食用菌学报,2018,25(1):1-12.Tan W, Miao RY, Zhou J, et al. Advances in cultivation techniques of Auricularia cornea[J]. Acta Edulis Fungi, 2018, 25(1):1-12.
[2]暴增海.植物生长调节剂对食用菌菌丝体和子实体的影响[J].浙江食用菌,1995,(3):6-8.Bao ZH. Effects of plant growth regulators on mycelium and fruiting bodies of edible fungi[J]. Zhejiang Edible Fungi, 1995,(3):6-8.
[3]司文帅,张颖,聂冬霞,等.液相色谱-串联质谱法测定糙皮侧耳中9种植物生长调节剂的残留量[J].食用菌学报2017, 24(2):38-43.Si WS, Zhang Y, Nie DX, et al. Determination of nine plant growth regulator residues in Pleurotus ostreatus fruit bodies using LC-MS/MS[J].Acta Edulis Fungi, 2017, 24(2):38-43.
[4]诸力,王晨,陈红平,等.超高效液相色谱-串联质谱法同时测定茶叶中11种植物生长调节剂及吡虫啉、啶虫脒的残留[J].分析化学,2017,45(4):529-536.Zhu L, Wang C, Chen HP, et al. Simultaneous determination of plant growth regulators and imidacloprid, acetamiprid in tea by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chin J Ana Chem, 2017,45(4):529-536.
[5] EU Pesticide database. http://ec.europa.eu/food/plant/pesticides/eupesticides-database. 2019-01-07[Z].
[6] Minister of Health, Labor and Welfare. Positive List System for Agricultural Chemical Residues in Foods.The Japan Food Chemical Research Foundation. http://www.ffcr.or.jp/zaidan/FFCRHOME.nsf/pages/MRLs-p. 2019-01-07[Z].
[7] GB 2763-2016食品安全国家标准食品中农药最大残留限量[S].GB 2763-2016 National food safety standard-Maximum residue limits for pesticides in food[S].
[8]US Environment Protection Agency. Tolerances and exemptions for pesticide chemical residues in food.https://www.ecfr.gov/cgi-bin/retrieveECFR?gp=1&SID=8835cb1c09428e600454aff5a52eae05&ty=HT ML&h=L&mc=true&r=PART&n=pt40.26.180#se40.26.180_1569.2019-01-07[Z].
[9]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.Hao J, Jiang J, Mao T, et al. Determination of 34 plant growth regulator residues in vegetable and fruit by QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry[J]. Food Sci, 2018,39(8):267-275.
[10]吴平谷,谭莹,张晶,等.分级净化结合气相色谱-质谱联用法测定豆芽中10种植物生长调节剂[J].分析化学,2014,42(6):866-871.Wu PG, Tan Y, Zhang J, et al. Determination of 10 plant growth regulators in bean sprouts by sequential cleaning-gas chromatography-mass spectrometry[J]. Chin J Anal Chem, 2014,42(6):866-871.
[11]黄何何,张婿,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.Huang HH, Zhang J, Xu DM, et al. Determination of 21 plant growth regulator residues in fruits by QuEChERS-high performance liquidchromatography-tandem mass spectrometry[J]. Chin J Chromatogr, 2014,32(7):707-716.
[12] Han PC, Kai LS, Chen CW, et al. Modified QuEChERS method for 24plant growth regulators in grapes using LC-MS/MS[J]. J Food Drug Anal,2007, 26(2):1-12.
[13]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.Zhang LW, Jiao GR, Wang K, et al. Simultaneous determination of 26kinds of plant growth regulator residues in fruits and vegetable by QuEChERS-high performance high performance chromatography-tandem mass spectrometry[J]. J Food Saf Qual, 2016, 7(7):2677-2689.
[14]张博华.固相萃取一高效液相色谱联用同时分析环境水体中四种喹诺酮类抗生素[D].泰安:山东农业大学,2016.Zhang BH. Simultaneous determination of 4 quinolones antibiotics in environmental water by SPME-HPLC[D]. Tai'an:Shandong Agricultural University, 2016.
[15] Cheng ZP, Dong FS, Xu J, et al. Atmospheric pressure gas chromatography quadrupole-time-of-flight mass spectrometry for simultaneous determination of fifteen organochlorine pesticides in soil and water[J]. J Chromatogr A, 2016, 1435:115-124.
[16] Goh SXL, Duarah A, Zhang LF, et al. Online solid extraction with liquid chromatography-tandem mass spectrometry for determination of estrogens and glucocorticoids in water[J]. J Chromatogr A, 2016, 1465:9-19.
[17] Erin C, Diane MW, Lu ZL, et al. Systematic and comprehensive strategy for reducing matrix effects in LC/MS/MS analyses[J]. J Chromatogr B,2007, 852:22-34.
[18]唐维英,黄泽玮,钱广生,等.超高效液相色谱-串联质谱法测定茶叶、代用茶和饮料食品中63种非法添加化合物[J].色谱,2018, 36(12):1245-1260.Tang WY, Huang ZW, Qian GS, et al. Determination of 63 compounds illegally added in tea, substitute tea and beverage foods by ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Chin J Chromatogr, 2018, 36(12):1245-1260.
[2]暴增海.植物生长调节剂对食用菌菌丝体和子实体的影响[J].浙江食用菌,1995,(3):6-8.Bao ZH. Effects of plant growth regulators on mycelium and fruiting bodies of edible fungi[J]. Zhejiang Edible Fungi, 1995,(3):6-8.
[3]司文帅,张颖,聂冬霞,等.液相色谱-串联质谱法测定糙皮侧耳中9种植物生长调节剂的残留量[J].食用菌学报2017, 24(2):38-43.Si WS, Zhang Y, Nie DX, et al. Determination of nine plant growth regulator residues in Pleurotus ostreatus fruit bodies using LC-MS/MS[J].Acta Edulis Fungi, 2017, 24(2):38-43.
[4]诸力,王晨,陈红平,等.超高效液相色谱-串联质谱法同时测定茶叶中11种植物生长调节剂及吡虫啉、啶虫脒的残留[J].分析化学,2017,45(4):529-536.Zhu L, Wang C, Chen HP, et al. Simultaneous determination of plant growth regulators and imidacloprid, acetamiprid in tea by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chin J Ana Chem, 2017,45(4):529-536.
[5] EU Pesticide database. http://ec.europa.eu/food/plant/pesticides/eupesticides-database. 2019-01-07[Z].
[6] Minister of Health, Labor and Welfare. Positive List System for Agricultural Chemical Residues in Foods.The Japan Food Chemical Research Foundation. http://www.ffcr.or.jp/zaidan/FFCRHOME.nsf/pages/MRLs-p. 2019-01-07[Z].
[7] GB 2763-2016食品安全国家标准食品中农药最大残留限量[S].GB 2763-2016 National food safety standard-Maximum residue limits for pesticides in food[S].
[8]US Environment Protection Agency. Tolerances and exemptions for pesticide chemical residues in food.https://www.ecfr.gov/cgi-bin/retrieveECFR?gp=1&SID=8835cb1c09428e600454aff5a52eae05&ty=HT ML&h=L&mc=true&r=PART&n=pt40.26.180#se40.26.180_1569.2019-01-07[Z].
[9]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.Hao J, Jiang J, Mao T, et al. Determination of 34 plant growth regulator residues in vegetable and fruit by QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry[J]. Food Sci, 2018,39(8):267-275.
[10]吴平谷,谭莹,张晶,等.分级净化结合气相色谱-质谱联用法测定豆芽中10种植物生长调节剂[J].分析化学,2014,42(6):866-871.Wu PG, Tan Y, Zhang J, et al. Determination of 10 plant growth regulators in bean sprouts by sequential cleaning-gas chromatography-mass spectrometry[J]. Chin J Anal Chem, 2014,42(6):866-871.
[11]黄何何,张婿,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.Huang HH, Zhang J, Xu DM, et al. Determination of 21 plant growth regulator residues in fruits by QuEChERS-high performance liquidchromatography-tandem mass spectrometry[J]. Chin J Chromatogr, 2014,32(7):707-716.
[12] Han PC, Kai LS, Chen CW, et al. Modified QuEChERS method for 24plant growth regulators in grapes using LC-MS/MS[J]. J Food Drug Anal,2007, 26(2):1-12.
[13]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.Zhang LW, Jiao GR, Wang K, et al. Simultaneous determination of 26kinds of plant growth regulator residues in fruits and vegetable by QuEChERS-high performance high performance chromatography-tandem mass spectrometry[J]. J Food Saf Qual, 2016, 7(7):2677-2689.
[14]张博华.固相萃取一高效液相色谱联用同时分析环境水体中四种喹诺酮类抗生素[D].泰安:山东农业大学,2016.Zhang BH. Simultaneous determination of 4 quinolones antibiotics in environmental water by SPME-HPLC[D]. Tai'an:Shandong Agricultural University, 2016.
[15] Cheng ZP, Dong FS, Xu J, et al. Atmospheric pressure gas chromatography quadrupole-time-of-flight mass spectrometry for simultaneous determination of fifteen organochlorine pesticides in soil and water[J]. J Chromatogr A, 2016, 1435:115-124.
[16] Goh SXL, Duarah A, Zhang LF, et al. Online solid extraction with liquid chromatography-tandem mass spectrometry for determination of estrogens and glucocorticoids in water[J]. J Chromatogr A, 2016, 1465:9-19.
[17] Erin C, Diane MW, Lu ZL, et al. Systematic and comprehensive strategy for reducing matrix effects in LC/MS/MS analyses[J]. J Chromatogr B,2007, 852:22-34.
[18]唐维英,黄泽玮,钱广生,等.超高效液相色谱-串联质谱法测定茶叶、代用茶和饮料食品中63种非法添加化合物[J].色谱,2018, 36(12):1245-1260.Tang WY, Huang ZW, Qian GS, et al. Determination of 63 compounds illegally added in tea, substitute tea and beverage foods by ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Chin J Chromatogr, 2018, 36(12):1245-1260.