ICP-MS法测定清火栀麦片及胶囊中25种元素的残留量

目的：应用电感耦合等离子体质谱技术（ICP-MS）建立同时测定清火栀麦片/胶囊中锂、钒、铬、铁、镍、钴、铜、锌、砷、硒、钼、钌、铑、钯、银、镉、锡、锑、钡、铱、铂、金、汞、铊、铅25种元素的方法，并建议限度要求。方法：微波程序升温消解法处理样品（片剂47批，胶囊剂2批），以72锗、115铟、209铋为内标，电感耦合等离子体质谱法测定清火栀麦系列制剂中25种元素的残留量。结果：各元素在各自的浓度范围内线性关系良好（r>0.999）；检测下限为0.000 3~5.2 μg·d^-1；回收率为88.1%~121.9%，RSD为0.7%~6.7%。参照USP 41-NF 36及EP 9.0拟定各元素残留限度，结果-2批片剂中铅的残留量超出拟定限度，且标示为同一厂家，1批胶囊中砷的残留量超出拟定限度，存在一定用药风险。结论：该方法简便、灵敏、准确，可用于清火栀麦片及胶囊中多种元素的检测，为其风险监控提供技术参考。

Objective:To establish a method for determination of 25 elements including Li,V,Cr,Fe,Ni,Co,Cu,Zn,As,Se,Mo,Ru,Rh,Pd,Ag,Cd,Sn,Sb,Ba,Ir,Pt,Au,Hg,Tl and Pb in Qinghuozhimai preparations(tablets and capsules)by inductively coupled plasma mass spectrometry(ICP-MS),and propose the limits.Methods:47 tablets and 2 capsules were digested by temperature programmed microwave digestion.25 elements were determined by ICP-MS with ⁷²Ge,¹¹⁵In and ²⁰⁹Bi as the internal standards.Results:The linearity was good for all elements with correlative coefficients(r)above 0.999.The limits of detections were in the range of 0.000 3 to 5.2 μg·d^-1.The recoveries of elements were between 88.1% and 121.9% with RSDs within 0.7% to 6.7%.According to the requirement of USP 41-NF 36 and EP 9.0,the residual of lead in 2 out of 47 tablets exceeded the prescribed limit and were labeled as the same manufacturer.The residue of arsenic in 1 of 2 capsules exceeded the prescribed limit.There was some risk of medication.Conclusion:The method is simple,sensitive and accurate,and it can be used for the determination of multiple elements in Qinghuozhimai preparations,providing helpful information for the risk monitoring.

[1] 中华人民共和国药典2015年版.一部[S].2015:1535 ChP 2015.Vol Ⅰ[S].2015:1535
[2] 车伟民.清火桅麦片致慢性腹泻2例[J].药物流行病学杂志,2006,15(6):323 CHE WM.2 cases of chronic diarrhea caused by Qinghuozhimai tablets[J].Chin J Pharmacoepidemiol,2006,15(6):323
[3] 马里,司惠芳.清火桅麦片致药疹1例[J].药物流行病学杂志,2005,14(2):112 MA L,SI HF.One case of drug eruption caused by Qinghuozhimai tablets[J].Chin J Pharmacoepidemiol,2005,14(2):112
[4] 张丽娟,谷学新,周勇义.中药产品中的重金属元素[J].首都师范大学学报(自然科学版),2004,25(1):34 ZHANG LJ,GU XX,ZHOU YY.Heavy metals in Chinese traditional medicines[J].J Cap Norm Univ:Nat Sci Ed,2004,25(1):34
[5] 孙艳,赵余庆.药食同源品中重金属的检测方法与思考[J].中草药,2011,42(11):2351 SUN Y,ZHAO YQ.Consideration and detection methods of heavymetals in medicinal and edible goods[J].Chin Tradit Herb Drugs,2011,42(11):2351
[6] CLARKSON TW,MAGOS L.The toxicity of mercury and its chemical compounds[J].Crit Rev Toxicol,2006,6(8):609
[7] CAUSSY D.Cause study of the impact of understanding bioavailability arsenic[J].Ecotoxicol Environ Saf,2003,56(1):164
[8] 聂黎行,张毅,戴忠,等.国家药品评价抽验对中药标准提高的促进作用[J].中国药业,2013,22(22):2 NIE LX,ZHANG Y,DAI Z,et al.National drug evaluation testing on the improvement of Chinese traditional medicine[J].China Pharm,2013,22(22):2
[9] 贾艾玲,王红梅,李玲玲.电感耦合等离子体质谱法检测阿胶中6种有害元素的含量[J].药物分析杂志,2012,32(3):434 JIA AL,WANG HM,LI LL.ICP-MS determination of 6 hazard elements in Colla Corii Asini(Ejiao)[J].Chin J Pharm Anal,2012,32(3):434
[10] 刘潇潇,杨德忠,李华.ICP-MS法测定清开灵系列制剂中17种元素的含量[J].药物分析杂志,2015,35(11):2018 LIU XX,YANG DZ,LI H.Content determination of 17 elements in Qingkailing preparations by ICP-MS[J].Chin J Pharm Anal,2015,35(11):2018
[11] USP 41-NF 36[S].2018:6147
[12] EP 9.0[S].2017:775
[13] 金红宇,戴博,田金改,等.中药中外源性有害残留物的控制[J]中国药事,2007,21(12):1013 JIN HY,DAI B,TIAN JG,et al.Control of extrinsic harmful residues in traditional Chinese medicine[J]Chin Pharm Aff,2007,21(12):1013