目的探究一種更加準(zhǔn)確、合理且對(duì)儀器影響較小的電感耦合等離子體質(zhì)譜（ICP-MS）重金屬檢測(cè)方法的在線內(nèi)標(biāo)物濃度。方法選擇標(biāo)準(zhǔn)曲線范圍內(nèi)10、50、200、500、1 000 μg/L的質(zhì)量濃度水平作為內(nèi)標(biāo)溶液在線加入,測(cè)定梔子藥材中V、Cr、Mn、Fe、Ni、Cu、Zn、As、Cd、Pb和Hg元素。結(jié)果低濃度水平內(nèi)標(biāo)不足以校正儀器波動(dòng),對(duì)測(cè)定結(jié)果影響較大；高濃度內(nèi)標(biāo)溶液易造成污染,在校正儀器的同時(shí)容易掩蓋信號(hào),影響進(jìn)樣前調(diào)諧；500 μg/L內(nèi)標(biāo)既能使待測(cè)元素有穩(wěn)定的響應(yīng)值,又不會(huì)過于抑制信號(hào)。結(jié)論內(nèi)標(biāo)濃度的選擇既要兼顧標(biāo)準(zhǔn)曲線進(jìn)樣濃度,又要避免濃度過高造成的信號(hào)掩蓋,500 μg/L的內(nèi)標(biāo)濃度能夠有效補(bǔ)償中藥材金屬元素測(cè)定過程的基體效應(yīng),測(cè)定結(jié)果相對(duì)準(zhǔn)確。

Objective To provide a proper concentration of Internal Standard Solution by comparing five different degrees to the simultaneous analysis of 10 metals including V, Cr, Mn, Fe, Ni, Cu, As, Cd, Pb and Hg in Cardenia jasminoides. Method An Inductively Coupled Plasma-Mass Spectrometry method with Microwave-Assisted Digestion was developed with 10, 50, 200, 500, 1 000 μg/L of Ge, In, Bi as internal standard. Result The degree of 500 μg/L concentration of internal stand solution can both correct the matrix effect and alleviate the contamination as the 1 000 μg/L. Conclusion With excellent detection limits, high sensitivity and wide linear range, the 500 μg/L internal standard may serve as reference in the determination of elements in other traditional Chinese medicine (TCM).