Zhai Yu-Yao, Guo Bao-Lin
Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences and Peking Union Medical College, Beijing 100193, China.
Xi'an No.4 Hospital, Xi'an 710004, China.
Zhongguo Zhong Yao Za Zhi. 2017 Jun;42(11):2110-2116. doi: 10.19540/j.cnki.cjcmm.20170223.024.
HPLC-MS/MS was applied to the determination of residual amount of plant growth retardant such as paclobutrazol, daminozide, chlormequat and mepiquat chloride in dried root and rhizome herbs. The sample was extracted twice with acetonitrile containing 0.1% formic acid. The separation was performed on a Waters Atlantis HILIC column with an elution system consisting of acetonitrile-5 mmol•L⁻¹ ammonium acetate solution with 0.1% formic acid, methanol and acetonitrile. The MS spectrum was acquired in positive mode with multiple reactions monitoring (MRM). The linear range was 6-1 500 μg•kg⁻¹, and the optimized method offered a good linear correlation (r>0.997 8), excellent precision (RSD<11%) and acceptable recovery (from 79.3% to 103.3%). Four kinds of plant growth retardant have detected in some ofhenise herbs like Ophiopogonis Radix, Angelicae Sinensis Radix, Achyranthis Bidentatae Radix, Alismatis Rhizoma, Chuanxiong Rhizama and Notoginseng Radix et Rhizama, is among the more severe cases, dwarf lilyturf, multi-effect azole detection quantity is 63.4~1 351.66 μg•kg⁻¹, and Daminozide was detected in Ophiopogonis Radix, Angelicae Sinensis Radix, Chuanxiong Rhizama, Alismatis Rhizoma.
采用高效液相色谱-串联质谱法(HPLC-MS/MS)测定了麦冬、当归、牛膝、泽泻、川芎、三七等根茎类药材中多效唑、丁酰肼、矮壮素、甲哌鎓等植物生长调节剂的残留量。样品用含0.1%甲酸的乙腈提取两次。采用沃特世Atlantis HILIC色谱柱,以乙腈-5 mmol•L⁻¹含0.1%甲酸的乙酸铵溶液、甲醇和乙腈组成的洗脱系统进行分离。质谱采用正离子模式,多反应监测(MRM)采集。线性范围为61 500 μg•kg⁻¹,该优化方法具有良好的线性相关性(r>0.997 8)、精密度高(RSD<11%)和回收率良好(79.3%103.3%)。在麦冬、当归、牛膝、泽泻、川芎、三七等一些根茎类药材中检测到了4种植物生长调节剂,情况较为严重,麦冬中多效唑的检测量为63.4~1 351.66 μg•kg⁻¹,丁酰肼在麦冬、当归、川芎、泽泻中均有检出。