| 引用本文: | 裘一婧,贾彦博,方玲,胡程,曾金林.超声酶水解提取/高效液相色谱-原子荧光光谱联用法测定动物源性中药中的砷形态[J].中国现代应用药学,2019,36(23):2943-2948. |
| QIU Yijing,JIA Yanbo,FANG Ling,HU Cheng,ZENG Jinlin.Determination of Arsenic Speciation by HPLC Combined with Atomic Fluorescence Spectrometry (HPLC-AFS) Using Ultrasound and Enzymatic Hydrolysis in Animal Derived Traditional Chinese Medicines[J].Chin J Mod Appl Pharm(中国现代应用药学),2019,36(23):2943-2948. |
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| 超声酶水解提取/高效液相色谱-原子荧光光谱联用法测定动物源性中药中的砷形态 |
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裘一婧1, 贾彦博1, 方玲2,3, 胡程1, 曾金林1
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1.杭州市食品药品检验研究院, 杭州 310022;2.浙江康恩贝制药股份有限公司, 杭州 310022;3.浙江省中药制药技术重点实验室, 杭州 310052
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| 摘要: |
| 目的 采用液相色谱-原子荧光光谱（HPLC-AFS）联用技术对动物源性中药中一甲基砷酸（monomethylarsine，MMA）、二甲基砷酸（dimethyarsine，DMA）、三价砷[As（Ⅲ）]、五价砷[As（V）]的形态进行研究。方法 样品中加入pH 2.5的胃蛋白酶液，于55℃超声20 min，6 000 r·min-1离心3 min，取其上清液，过滤进样。采用Hamilton PPRP-X100阴离子交换色谱柱（150 mm×4.6mm，5 μm）分离，1 mmol·L-1磷酸二氢铵溶液（pH 8.5），20 mmol·L-1磷酸二氢铵溶液（pH 7.0）体系组成的流动相按一定比例进行梯度洗脱，流速为1.0 mL·min-1，进样量为100 μL。结果 4种砷形态在13 min内完成分离。MMA、DMA、As（Ⅲ）、As（V）的检出限分别为0.01，0.01，0.01和0.02 mg·kg-1，样品中加标量为0.03~0.1 mg·kg-1时，4种砷化合物的回收率为93.4%~105.4%，精密度RSD为0.8%~4.4%。结论 本研究建立的超声酶水解提取/HPLC-AFS测定动物源性中药中砷形态的分析方法样品提取简便，提取率高，测定方法精密度好，准确度高。 |
| 关键词: 砷形态 高效液相色谱-原子荧光联用 动物源性中药 |
| DOI：10.13748/j.cnki.issn1007-7693.2019.23.012 |
| 分类号:R917.101 |
| 基金项目: |
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| Determination of Arsenic Speciation by HPLC Combined with Atomic Fluorescence Spectrometry (HPLC-AFS) Using Ultrasound and Enzymatic Hydrolysis in Animal Derived Traditional Chinese Medicines |
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QIU Yijing1, JIA Yanbo1, FANG Ling2,3, HU Cheng1, ZENG Jinlin1
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1.Hangzhou Institute for Food and Drug Control, Hangzhou 310022, China;2.Zhejiang CONBA Pharmaceutical Co., Ltd., Hangzhou 310022, China;3.Zhejiang Provincial Key Laboratory of TCM Pharmaceutical Technology, Hangzhou 310052, China
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| Abstract: |
| OBJECTIVE To develop a method to determine four arsenic(As) speciation including arsenite[As(Ⅲ)], arsenate[As(V)], monomethylarsine(MMA), dimethyarsine(DMA) by HPLC-AFS using ultrasound and enzymatic hydrolysis in animal derived traditional Chinese medicines. METHODS Add pepsin to the samples after ultrasound and enzymatichydrolysis (pH 2.5) with 55℃ for 20 min, centrifuged at 6 000 r·min-1 for 3 min. Took the supernatant, filter the sample. The sample was separated on an Hamilton PPRP-X100 anion exchange column(150 mm×4.6 mm, 5 μm) with the mobile phase of 1 mmol·L-1 NH4H2PO4(pH 8.5) and 20 mmol·L-1 NH4H2PO4(pH 7.0) by the gradient elution. The flow rate was 1.0 mL·min-1 and the injection volume was 100 μL. RESULTS The separation was achieved within 13 min for four arsenic speciations. The detect limits were 0.01, 0.01, 0.01 and 0.02 mg·kg-1 for MMA, DMA, As(Ⅲ) and As(V) respectively. The recoveries of four arsenic speciations ranged from 93.4% to 105.4%, the RSDs of precision were among 0.8% to 4.4% with the spiked amounts of 0.03-0.1 mg·kg-1 in the samples. CONCLUSION The developed HPLC-AFS method using ultrasound and enzymatic hydrolysis for determination of As speciation has the advantages of simplicity, high extraction rate, good precision and high accuracy. |
| Key words: arsenic speciation HPLC-AFS animal derived traditional Chinese medicines |
