目的 建立微波消解-ICP-MS方法并测定注射用红花黄色素、注射用灯盏花素、注射用尿激酶、注射用鹿瓜多肽、注射用血塞通、注射用双黄连、痰热清注射液、丹参滴注液、银杏达莫注射液、丹红注射液中13种金属元素(Pb、Cd、Hg、As、Cu、Fe、Mn、Ba、Zn、Al、Co、Cr、Ni)。方法 HNO₃和H₂O₂作为消解酸体系,采用微波消解法前处理样品后,以Sc、In、Rh、Re作为内标,通过ICP-MS法同时测定注射剂中13种金属元素的量。结果 各元素线性关系均良好(r> 0.999),方法检出限为0.008～0.069 μg/L,平均回收率为93.61%～100.79%,精密度和重复性的RSD值均小于5%;10种中药注射剂中的Cd和As均小于检出限,Pb为0.017～0.109 mg/kg,Cu为0.016～0.135 mg/kg,Hg为0.005～0.018mg/kg,Fe为0.335～2.081 mg/kg,Mn为0.021～0.699 mg/kg,Ba为0.009～0.028 mg/kg,Zn为0.005～3.186 mg/kg,Al为0.518～10.012 mg/kg,Co为0.003～0.028 mg/kg,Cr为0.006～0.179 mg/kg,Ni为0.005～1.187 mg/kg,5种明确需要控制的有害重金属元素(Pb、Cd、Hg、As、Cu)的残留量符合《中国药典》2010年版规定,其他Fe、Mn、Zn、Al等金属元素的安全限量有待进一步深入研究分析。结论 本研究所建立的方法具有简便、快速、准确、灵敏度高的优点,可推荐用于中药注射剂中金属元素的定量测定并为其质量监控提供参考。

Objective To establish microwave digestion-inductively coupled plasma mass spectrometry (ICP-MS) method for the determination of 13 kinds of metals (Pb, Cd, Hg, As, Cu, Fe, Mn, Zn, Ba, Al, Co, Cr, and Ni) in 10 kinds of Chinese materia medica (CMM) injections which are Carthamin yellow for injection, Breviscapine for injection, Urokinase for injection, Lugua Polypeptide for injection, Xuesetong for injection, Shuanghuanglian for injection, Tanreqing Injection, Salvia miltiorrhiza Injection, Yinxing Damo Injection, and Danhong Injection). Methods HNO₃ and H₂O₂ are as acid digestion system; Samples were conducted pretreatment by microwave digestion instrument; Sc, In, Rh, and Re were used as internal standard elements, 13 kinds of elements were determined by ICP-MS at the same time. Results Different kinds of the elements had a good linear relationship (r > 0.999); The limit of detection was range from 0.008 to 0.069 μg/L, the average recovery rate was range from 93.61% to 100.79%; RSD values of the repeatability and precision were all less than 5%, The As and Cd in 10 kinds of CMM injections were all less than the limit of detection, Pb was ranged from 0.109 to 0.017 mg/kg, Cu was ranged from 0.016 to 0.135 mg/kg, Hg was ranged from 0.005 to 0.018 mg/kg, Fe was ranged from 0.335 to 2.081 mg/kg, Mn was ranged from 0.021 to 0.699 mg/kg, Ba was ranged from 0.009 to 0.028 mg/kg, Zn was ranged from 0.005 to 3.186 mg/kg, Al was ranged from 0.518 to 10.012 mg/kg, Co was ranged from 0.003 to 0.028 mg/kg, Cr was ranged from 0.006 to 0.179 mg/kg, Ni was ranged 0.005 to 1.187 mg/kg, five kinds of heavy metals which were needed to control were safe according to Chinese Pharmacopoeia (2010), the contents of Fe, Mn, Zn, and Al were not too high, but their safe limits were needed to be further in-depth researched and analyzed. Conclusion This method is simple and fast, and has good accuracy and high precision, so it can be recommended for the determination of metal elements in CMM injections and provide the reference for its quality control.

中英联合项目(合同)