加味逍遥方10味药材及其提取物中18种有毒害元素的含量测定及其转移率研究  

Study on Contents Determination and Transport Rates of 18 Toxic Elements from 10 Ingredients of Modified Xiaoyao Formula and Their Extracts

作　　者：张雅丽[1,2] 孙巍[2] 张磊[2] 毛明朋 叶正良[3] 

机构地区：[1]天津中医药大学中药学院,天津300193 [2]天士力制药集团股份有限公司,天津300402 [3]天士力控股集团有限公司,天津300402

出　　处：《中国药房》2017年第18期2564-2568,共5页China Pharmacy

摘　　要：目的:建立同时测定加味逍遥方10味药材及其提取物中18种有毒害元素含量的方法,并研究上述元素的转移率。方法:采用微波消解-电感耦合等离子体质谱法。射频功率为1.50 k W,雾化气压力为720 k Pa,采样深度为7 mm,等离子气体流速为15.0 L/min,载气流速为1.00 L/min,雾化室温度为2℃,氦气流速为4.5 m L/min,测量点数/峰为3,数据采样模式为跳峰采集。结果:砷(As)、铅(Pb)、铜(Cu)、汞(Hg)、镉(Cd)、钼(Mo)、钒(V)、铬(Cr)、锰(Mn)、铁(Fe)、镍(Ni)、锌(Zn)、钌(Ru)、铑(Rh)、钯(Pd)、锇(Os)、铱(Ir)、铂(Pt)检测进样量线性范围为0~500.17 ppb(r为0.999 4~0.999 9);检测限为0.000 4~5.341 0 ng/g;重复性试验的RSD<5.0%;平均加样回收率为82.0%~117.9%(RSD为0.2%~5.7%,n=9)。Ru、Rh、Pd、Os、Ir、Pt、Hg未在药材和提取物中检出,其余11种元素在提取物中的转移率为1.46%~31.90%。结论:该方法操作简便,精密度、稳定性、重复性好,可用于加味逍遥方中10味药材及其提取物中18种有毒害元素含量的同时测定。加味逍遥方提取物在制备过程中降低了有毒害元素的含量,可在一定程度上保证用药的安全性。OBJECTIVE： To establish a method for simultaneous determination of 18 toxic elements from 10 ingredients of Modified xiaoyao formula and their extracts, and to study transport rates of above elements. METHODS ： Microwave digestion-inductively coupled plasma mass （ICP-MS） was used to determine above elements. Radio-frequency power was 1.50 kW, atomization pressure was 720 kPa, sampling depth was 7 mm, plasma gas flow rate was 15.0 L/min, carrier gas flow rate was 1.00 L/min, spray chamber temperature was 2 ℃, He flow rate was 4.5 mL/min under collision mode, measurement points/peak was 3, data acquisition mode was jump mode. RESULTS. The linear ranges of As, Pb, Cu, Hg, Cd, Mo, V, Cr, Mn, Fe, Ni, Zn, Ru, Rh, Pd, Os, Ir, Pt was 0-500.17 ppb（r was 0.999 4-0999 9）; LOD was 0.000 4-5.341 0 ng/g; RSD of repeatability tests was all lower than 5.0%; average recoveries were 82.0%-117.9% （RSD=0.2%-5.7% ,n=9）. Ru, Rh, Pd, Os, Ir, Pt, Hg had not been detected. The transfer rates of 11 metals in the extracts ranged 1.46%-31.90%. CONCLUSIONS： The method is simple, precise, stable and repeatable, and can be used for simultaneous determination of 18 toxic elements in 10 ingredients of Modified xiaoyao formula and their extracts. The contents of toxic elements are decreased during the preparation of Modified xiaoyao formula extract to guarantee the safety of drug use to certain extent.

关 键 词：加味逍遥方 转移率 电感耦合等离子体质谱法 药材 提取物 

分 类 号：R927[医药卫生—药学]