尿素［¹³C］呼气试验诊断试剂盒中掺杂尿素的快速GC/MS检测

目的： 建立尿素[¹³C]呼气试验诊断试剂盒中掺杂尿素的快速检测方法。方法： 采用气相色谱-质谱联用法，色谱柱为Thermo TG-WAXMS A（15 m×0.25 mm×0.25 μm），单四极杆EI离子源进行检测，选择离子扫描模式。结果： 2%~50%的尿素加样测定理论值与实际值误差小于0.4%，3批实际样品经检测未添加普通尿素。该检测方法的定量下限为0.25 mg·mL^-1，在0.1~1 mg·mL^-1的线性范围内，尿素[¹³C]对照品的¹³C丰度均值为99.0%（n=6，RSD=0.090%）。结论： 该方法操作简便快速、灵敏可靠，适用于尿素[¹³C]呼气试验诊断试剂盒中掺杂普通尿素的快速检测。

Objective: To develop a rapid method for the determination of urea in urea[¹³C] breath test kit. Methods: The method was based on gas chromatography-mass spectrometry (GC-MS). The column was Thermo TG-WAXMS A (15 m×0.25 mm×0.25 μm)and detection was performed on a single quadruple EI ion source,scanning m/z 59-63 was detected by selective ion monitoring mode to calculate the ¹³C abundance. Results: In the range of 2% to 50% urea addition to the sample,the measurement error was lower than 0.4%. Three urea[¹³C] breath test kits were demonstrated no urea addition. The limit of quantification was 0.25 mg·mL^-1. In the range of 0.1-1 mg·mL^-1,the mean abundance of ¹³C of UREA C13 USP reference standard was 99.0%(n=6,RSD=0.090%). Conclusion: The method is simple,rapid,sensitive and reliable. It is suitable for rapid testing of urea in urea[¹³C]breath test kit.

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