Objective: To establish an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) combined with standard addition method for the determination of paclobutrazol residues in Shengmai injection, Shenmai injection and Yiqi Fumai injection (freeze-dried). Methods: Thermo Hypersil Gold column (100 mm×2.1 mm, 1.9μm) was used for gradient elution with 0.1% formic acid solution and methanol as mobile phase. Electrospray ionization (ESI) and multiple reaction monitoring (MRM) in positive ion mode were applied. Standard addition method was used in sample pretreatment. Results: The linear relationship of the method was good, and the correlation coefficients were greater than 0.998. The recoveries were in the ranges of 94.5%-119.8%, RSD was in the range of 1.4%-2.5%, and the lower limit of detection was in the range of 0.7-0.8 ng·mL-1. A total of 47 batches of samples were screened, of which 85% were not detected with paclobutrazole, which was generally safe and controllable. However, paclobutrazole was detected in some batches of samples in all three injections, which had a certain safety risk. Conclusion: The standard addition method can effectively overcome matrix effect and is easy to operate. The method is sensitive, accurate and reliable.
[1] 贾洪涛. 植物生长延缓剂——多效唑[J]. 农技服务,2004(1):60
JIA HT. A plant growth regulator——paclobutrazol[J]. Agric Technol Serv, 2004(1):60
[2] 李敏,付桂平,吕宁,等. EPA内分泌干扰物研究进展[J]. 农药科学与管理,2016,37(4):16
LI M, FU GP, LÜ N, et al. Research progress of EPA endocrine disruptors[J]. Pestic Sci Admin, 2016,37(4):16
[3] 程燕,谭丽超,周军英,等. 我国环境激素类农药优先名录筛选[J]. 农药科学与管理,2014,35(4):28
CHENG Y,TAN LC,ZHOU JY, et al. Screening of the priority list of pesticide endocrine disruptors in China [J]. Pestic Sci Admin,2014,35(4):28
[4] 中华人民共和国国家标准.食品安全国家标准, 食品中农药最大残留限量(GB2763-2021) [S]. 2021:102
National Standards of The People’s Republic of China. National Standard for Food Safety, Maximum Residue Limits for Pesticides in Food (GB2763-2021) [S]. 2021:102
[5] Amending Annexes Ⅱ, Ⅲ and Ⅴ to Regulation (EC) No 396/2005 of the European Parliament and of the Council as Regards Maximum Residue Levels for Bromadiolone, Etofenprox, Paclobutrazol and Penconazole in or on Certain Products. Commission Regulation (EU) [S]. 2019
[6] 余翠翠, 王晖, 隋春, 等. 四川三台麦冬产区生长调节剂使用情况调研及残留研究[J]. 中国现代中药,2019,21(12):1669
YU CC, WANG H, SUI C, et al. Study on application and residue analysis of plant growth regulator in Ophiopogon japonicus in Santai County of Sichuan Province [J]. Mod Chin Med, 2019,21(12):1669
[7] 吴东明, 李怡, 邓晓, 等. 高效液相色谱法测定多效唑在海南芒果园土壤的吸附特征[J]. 农业资源与环境学报, 2020, 37(5):777
WU DM, LI Y, DENG X, et al. Characteristics of paclobutrazol sorption in mango soil in Hainan Province using high performance liquid chromatography [J] . J Agric Res Environ, 2020, 37(5):777
[8] 周勇, 刘佳, 朱航, 等. QuEChERS结合高效液相色谱串联质谱法测定柑橘中多效唑残留量[J]. 食品安全质量检测学报, 2020, 11(15):4995
ZHOU Y, LIU J, ZHU H, et al. Determination of paclobutrazol residue in citrus by QuEChERS-high performance liquid chromatography-tandem mass spectrometry [J]. J Food Saf Qual Test, 2020, 11(15):4995
[9] 欧阳秋丽. 食品中烯效唑和多效唑免疫分析新方法研究[D]. 南昌:南昌大学, 2020
OUYANG QL. New Study on Immunoassay Methods of Paclobutrazole and Enobutrazole in Food [D]. Nanchang: Nanchang University, 2020
[10] 李瑞瑆. 麦冬中农药残留风险评估及多效唑对其品质影响研究[D]. 北京:中国农业科学院, 2020
LI RX. Risk Assessment of Pesticide Residues and Effect of Paclobutrazole on Its Quality of Ophiopogon japonicus[D]. Beijing: Chinese Academy of Agricultural Sciences, 2020
[11] 陶玲, 李红彦, 陈华林, 等. 基于药材性状、产量及有效成分含量综合评价多效唑对麦冬质量的影响[J]. 中药材, 2019, 42(10):2231
TAO L, LI HY, CHEN HL, et al. To evaluate the effect of paclobutrazole on the quality of Ophiopogon japonicus based on medicinal characteristics, yield and active ingredient content[J]. J Chin Med Mater, 2019, 42(10):2231
[12] 苟琰, 高驰, 邓晶晶,等. QuEChERS结合GC-MS/MS-内标法测定川麦冬中多效唑残留量[J]. 中国药房,2019,30(3):323
GOU Y, GAO C, DENG JJ, et al. Determination of paclobutrazol residue in Ophiopogon japonicus from Sichuan by the QuEChERS combined with GC-MS/MS-internal standard detection[J]. Chin Pharm,2019,30(3):323
[13] 苏萌, 艾连峰. 液相色谱-串联质谱基质效应及其消除方法[J]. 食品安全质量检测学报, 2014, 5(2):511
SU M,AI LF. Matrix effects and elimination methods of liquid chromatography-tandem mass spectrometry [J]. J Food Saf Qual Test, 2014, 5(2):511
[14] 王立琦, 贺利民, 曾振灵, 等. 液相色谱-串联质谱检测兽药残留中的基质效应研究进展[J]. 质谱学报, 2011, 32(6):321
WANG LQ, HE LM, ZENG ZL, et al. Progress in matrix effect of veterinary drug residues analysis by high-performance liquid chromatography tandem mass spectrometry[J]. J Chin Mass Spectr Soc, 2011, 32(6):321
[15] 向平, 沈敏, 卓先义. 液相色谱-质谱分析中的基质效应[J]. 分析测试学报, 2009, 28(6):753
XIANG P, SHEN M, ZHUO XY. Matrix effects in liquid chromatographic-mass spectrometric analysis [J]. J Instrm Anal,2009, 28(6):753
[16] 黄宝勇, 欧阳喜辉, 潘灿平. 色谱法测定农产品中农药残留时的基质效应[J]. 农药学学报,2005,7(4):299
HUANG BY, OUYANG XH, PAN CP. Matrix effects in the analysis of pesticide residue in agro-products by chromatographic methods[J]. Chin J Pestic Sci,2005,7(4):299
[17] 刘晓云, 陈笑艳, 钟大放. 液相色谱-串联质谱生物分析方法的基质效应和对策[J]. 质谱学报, 2017, 38(4):388
LIU XY, CHEN XY, ZHONG DF. Matrix effects and countermeasure of liquid chromatography-tandem mass spectrometry in bioanalysis[J]. J Chin Mass Spectr Soc, 2017, 38(4):388
[18] 段醒妹, 张晔. 基质效应及其消除[J]. 赤峰学院学报(自然科学版), 2008, 96(8):17
DUAN XM, ZHANG Y. Matrix effects and their elimination[J]. J Chifeng Univ (Nat Sci Ed), 2008, 96(8):17
[19] 中华人民共和国药典2020年版.四部[S]. 2020:41
ChP 2020.Vol Ⅳ[S]. 2020:41
