气相色谱法测定细辛脑中的有机溶剂残留量

目的 建立气相色谱法测定细辛脑中四氢呋喃、乙醇、甲苯的残留量。方法 采用SUPELCOWAX-10的毛细管石英色谱柱（30mm×0．53mm，1．0μm）；载气：氮气；以N，N-二甲基甲酰胺为溶剂；柱温：60℃，保持5min，以30℃·min^-1。升温至180℃，维持1min；进样口温度：250℃；检测器温度：250℃（FID）。结果 四氢呋喃在0．634～211．2μg·mL^-1内线性关系良好，r＝0．999 1 （n＝6），最低检测限为0．190μg·mL^-1，回收率为98．8％（RSD=4．3％）；乙醇在1．032～206．4μg·mL^-1内线性关系良好，r＝0．9992（n＝6），最低检测限为0．310μg·mL^-1,回收率为97．7％（RSD=3．O％）；甲苯在0．604～36．24μg·mL^-1内线性关系良好，r＝0．9995（n＝6）），最低检测限为0．174μg·mL^-1，回收率为100．3％（RSD＝0．7％）：结论本方法可用于细辛脑中四氢呋喃、乙醇和甲苯的残留量测定。

Determination of residual solvents in asarone by GC

Objective To develop a gas chromatographic method and to determine the contents of residual organic solvents-tetrahydrofuran, ethanol, and toluene in asarone. Methods SUPELCOWAX-10 capillary column and FID detector were used. N, N-dimethylformamide was used as the solvent. The oven temperature started at 60 ℃. After 5 min, the temperature was programmatically increased to 180 ℃ at the rate of 30 ℃ per min and maintained for 1 min. The injection port temperature was 250 ℃ and the detector temperature was 250 ℃. Results The linear ranges of tetrahydrofuran, ethanol, and toluene were 0. 634～211.2μg· mL^-1 , 1. 032～206.4μg ·mL^-1 and 0. 580～36.24 μg · mL^-1 , respectively. The recovery of tetrahydrofuran, ethanol, and toluene was 95.1% （RSD=2.9%）, 100.6% （RSD=2.2%）,and 99.6% （RSD=1. 1%）, respectively. The detection limits of tetrahydrofuran, ethanol, and toluene were 0. 190 μg·mL^-1 , 0. 310μg ·mL^-1 and 0. 174μg · mL^-1 , respectively. Conclusion This method can be used to determine the organic volatile solvents of tetrahydrofuran, ethanol, and toluene in asarone.