Urine treatment method and method for detection of methylmalonic acid in urine by gas chromatography-mass spectrometry
A technique of urine methylmalonic acid and gas chromatography, applied in the directions of measuring devices, instruments, scientific instruments, etc., can solve the problems of difficult diagnosis, nerve damage, delayed treatment timing, etc., and achieves simple and easy operation and high accuracy and accuracy, the effect of saving sample processing time
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Embodiment 1
[0050] The processing of embodiment 1 urine
[0051] The urine of normal neonates and children with methylmalonic acidemia was collected, and processed according to the following steps: (1) the creatinine content in the urine was measured by ultraviolet spectrophotometry, and a urine sample equivalent to 0.2 mg of creatinine was taken; 2) Add the internal standard 2-phenyl-3-hydroxypropionic acid (tropic acid) and 2.0ml of frozen absolute ethanol, fully oscillate and mix evenly with an automatic vibrator; (3) Centrifuge at 4000rpm for 5 minutes to remove protein; (4) transfer the supernatant, and blow it with a nitrogen blower until it is completely dry at 60°C; (5) add bis(trimethylsilyl) tris to the dry residue at 70°C Fluoroacetamide (BSTFA): trimethylchlorosilane (TMCS) 99:1 silylating reagent for 30 minutes derivatization reaction. The whole process takes about 1 hour.
Embodiment 2
[0054] Embodiment 2 detects the processed urine
[0055] The urine sample pre-treated as above is detected by the existing GC-MS urine organic acid detection method and the GC-MS urine methylmalonic acid detection method of the present invention.
[0056] The instrument conditions of the existing GC-MS urine organic acid detection method are as follows:
[0057] 1. GC part
[0058] Injection mode: split mode;
[0059] Split ratio: 10:1;
[0060] Injection port temperature: 280°C;
[0061] Heating program: keep at 100°C for 4 minutes, raise to 280°C at a rate of 4°C / min, and hold for 11 minutes
[0062] Flow control mode: constant line speed;
[0063] 2. MS part
[0064] Ion source temperature: 200°C;
[0065] Interface temperature: 280°C;
[0066] Sampling method: Scan;
[0067] Interval: 0.50s;
[0068] Scan speed: 1000;
[0069] start m / z: 50;
[0070] End m / z: 500.
[0071] The detected spectrum is as figure 1 and figure 2 as shown, figure 1 For the results o...
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