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电感耦合等离子体质谱法测定明目上清片中5种元素含量

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目的 建立测定明目上清片中 5 种元素含量的电感耦合等离子体质谱(ICP-MS)法.方法 使用微波消解仪对样品进行预处理,等离子体射频功率为 1550 W,采样深度为 8.0 mm,等离子气体流速为 15 L/min,雾化气流速为 1.0 L/min,辅助气流速为 0.9 L/min,蠕动泵转速为 0.1 r/s.结果 铅、镉、砷、汞、铜元素质量浓度分别在 4~100 ng/mL、0.2~5 ng/mL、2~50 ng/mL、0.2~5 ng/mL、20~500 ng/mL范围内与仪器响应值线性关系良好(R2>0.9995,n=6);精密度、重复性试验结果的RSD均小于 4.0%;平均加样回收率分别 91.97%,104.12%,107.05%,92.74%,103.46%,RSD均小于 4.0%(n=6).4 家生产企业 34 批样品检出 5 种元素含量分别为 0.21~2.64,0.03~0.16,0.20~12.14,0.00~1.14,2.33~6.21 mg/kg.按拟订的限度(分别为 1.6,1.0,3.8,0.7,625 mg/kg),共有 2 批样品(涉及 2 家生产企业)存在超标现象,不合格率为 5.88%.结论 所建立的方法操作简单、快速、灵敏,结果准确,适用于明目上清片中 5 种元素的含量测定.
Determination of Five Elements in Mingmu Shangqing Tablets by ICP-MS
Objective To establish an inductively coupled plasma-mass spectrometry(ICP-MS)method for determining the contents of five elements in Mingmu Shangqing Tablets.Methods The samples were pretreated by a microwave digestion instrument.The plasma radio frequency power was 1550 W,the sampling depth was 8.0 mm,the plasma gas flow rate was 15 L/min,the atomization gas flow rate was 1.0 L/min,the auxiliary gas flow rate was 0.9 L/min,and the peristaltic pump speed was 0.1 r/s.Results The linear ranges of lead(Pb),cadmium(Cd),arsenic(As),mercury(Hg)and copper(Cu)were 4-100ng/mL,0.2-5ng/mL,2-50ng/mL,0.2-5ng/mL,20-500ng/mL(R2>0.9995,n=6)respectively.The RSDs of precision and repeatability tests were lower than 4.0%.The average recovery rates of the above five elements were 91.97%,104.12%,107.05%,92.74%,103.46%respectively,with RSDs lower than 4.0%(n=6).Pb,Cd,As,Hg and Cu were detected in 34 batches of samples from four manufacturing enterprises,with concentrations of 0.21-2.64,0.03-0.16,0.20-12.14,0.00-1.14,2.33-6.21 mg/kg respectively.According to the proposed limits(1.6,1.0,3.8,0.7,625 mg/kg),the element contents of two batches of samples(involving two manufacturing enterprises)were over the limit,with a disqualification rate of 5.88%.Conclusion The established method is simple,fast,sensitive and accurate,which is suitable for the determination of the five elements in Mingmu Shangqing Tablets.

Mingmu Shangqing Tabletstrace elementinductively coupled plasma-mass spectrometrycontent determination

池文杰

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福建省食品药品质量检验研究院,福建 福州 350012

明目上清片 微量元素 电感耦合等离子体质谱法 含量测定

2024

中国药业
重庆市食品药品监督管理局

中国药业

CSTPCD
影响因子:1.369
ISSN:1006-4931
年,卷(期):2024.33(16)
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