基于HPLC和UHPLC-MS/MS方法探究植物生长调节剂对白术品质的影响

Effect of Plant Growth Regulators on the Quality of Baizhu(Atractylodes Macrocephala Koidz.)by HPLC and UHPLC-MS/MS

目的:通过比较白术内在成分含量的变化及检测农药残留,探究植物生长调节剂的使用对白术品质产生的影响。方法:通过田间试验分别喷施不同浓度多效唑(A组)、矮壮·甲哌鎓(B组),并设计空白对照组(C组),收集样品;建立HPLC方法,同时测定白术中白术内酯Ⅰ、Ⅱ、Ⅲ及苍术酮的含量,比较A组、B组与C组的成分含量差异;建立UHPLC-MS/MS方法,同时检测白术中多效唑、矮壮素等8种植物生长调节剂的残留量,分析白术样品的残留情况。结果:HPLC测定白术内酯Ⅰ、Ⅱ、Ⅲ和苍术酮的含量,结果显示A组和B组的白术内酯Ⅰ、Ⅱ、Ⅲ含量均降低,且部分样品含量降低差异有统计学意义(P<0.01),A组的苍术酮含量先升高后降低,当多效唑浓度最高时,样品A5的苍术酮含量最低,且与C组比较,差异有统计学意义(P<0.01);B组的苍术酮含量变化程度不一。UHPLC-MS/MS检测结果显示,样品共检测出3种植物生长调节剂,分别为矮壮素、多效唑和烯效唑。白术A组多效唑残留量在2.81~246.67μg/kg;白术B组中矮壮素残留量在1.36~16.13μg/kg。白术A组多效唑的残留量和B组中矮壮素的残留量显著高于C组,且随着浓度的增加,残留量呈增大趋势。结论:白术种植过程中使用植物生长调节剂不但降低白术内在质量,还会使药材出现一定程度的有害残留,降低白术药材的安全性、有效性,进而可能会影响其临床用药,因此建议科学监管植物生长调节剂在白术种植过程中的使用。

Objective:To explore the effect of plant growth regulators on the quality of Baizhu(Atractylodes macrocephala Koidz.)by comparing the changes of internal components and detecting pesticide residues.Methods:Different concentrations of Paclobutrazol(group A),Chlormequat·Mepiquat chloride(group B)and blank control group(group C)were sprayed through field experiments to collect samples.A HPLC method was established for the simultaneous determination of Atractylenolide I,II,III and Atractylon in Baizhu(Atractylodes macrocephala Koidz.),and the difference of component content was compared among group A,group B and group C.UHPLC-MS/MS method was established for the simultaneous determination of eight plant growth regulator residues in Baizhu(Atractylodes macrocephala Koidz.),such as Paclobutrazol and Chlormequat chloride and so on.Results:The contents of Atractylenolide I,II,III and Atractylon were determined by HPLC.The results showed that the contents of Atractylenolide I,II,III decreased in group A and group B,and the content of some samples decreased significantly(P<0.01).The content of Atractylon in group A increased first and then decreased.When the concentration of Paclobutrazol was the highest,the content of Atractylon in sample A5 was the lowest.There was a significant difference compared with group C(P<0.01),while the content of Atractylon in group B varied.The results of UHPLC-MS/MS showed that three plant growth regulators were detected in the samples,namely Chlormequat chloride,Paclobutrazol and Uniconazole.The residual amount of Paclobutrazol was 2.81~246.67μg/kg in group A.The residual amount of Chlormequat chloride was 1.36~16.13μg/kg in group B.The residual amount of Paclobutrazol in group A and the residual amount of Chlormequat in group B were significantly higher than those in group C,and with the increase of concentration,the residual amount showed an increasing trend.Conclusion:The use of plant growth regulators in the planting process of Baizhu(Atractylodes macrocephala Koidz.),not only reduces the quality,but also produces more pesticide residues in the medicinal materials,which reduces the safety and effectiveness of Baizhu(Atractylodes macrocephala Koidz.)medicinal materials,and may affect its clinical medication.It is recommended to scientifically supervise the use of plant growth regulators in the planting process of Baizhu(Atractylodes macrocephala Koidz.).